Questo lavoro è stato supportato dalla nazionale natura Science Foundation of China (21301104), i fondi di ricerca fondamentali per le Università centrale (FRF-TP-16-019A3) e lo stato chiave laboratorio di ingegneria chimica (SKL--14A04).

1. sintesi di Mono-(2,3-dimethylbutyl) Acido fosfinico 18 , 19 <ol><li>reazione <ol><li>pesare 31,80 g idrato ipofosfito di sodio, ore 16.00 g di acido acetico, 8,42 g 2,3-dimetil-1-butene, 0,73 g di - tert-butylnperoxide (DTBP) e g 25,00 tetraidrofurano (THF) in autoclave a 100 mL in acciaio inox rivestito in Teflon, mettere un agitatore magnetico in autoclave e sigillare it.</li>
		<li>Mettere l'autoclave in un forno tubolare verticale che sotto il quale è un stirringapparatus magnetico. Avviare il mescolatore magnetico e impostare la velocità a 800 giri/min.</li>
		<li>Impostare il programma di riscaldamento del termoregolatore collegato all'autoclave: riscaldare da temperatura ambiente a 120 ° C durante 90 min, mantenere a 120 ° C per 8 h, poi raffreddare a temperatura ambiente, naturalmente. Avviare il programma di riscaldamento.</li>
	</ol></li> <li>Post-trattamento <ol><li>trasferire i prodotti in un pallone a sfondo sferico uno-collo 250 mL, lavare il rivestimento in Teflon con 50 mL di THF e aggiungerlo nel pallone stesso per garantire che tutti i prodotti vengono trasferiti.</li>
		<li>Rimuovere il THF e olefine non reagite utilizzando un evaporatore rotante.</li>
		<li>Trasferire il residuo in un imbuto separatore da 250 mL, lavare il matraccio con etere etilico 80 mL e 30 mL di acqua deionizzata rispettivamente e aggiungerli nell'imbuto stesso per garantire che tutti i prodotti vengono trasferiti.</li>
		<li>Aggiungere 50 mL della soluzione di NaOH 4% nell'imbuto sopra, agitare vigorosamente e separare la fase acquosa. Estrarre la fase organica con soluzioni di NaOH 4% 20 mL per tre volte (20 mL × 3) per assicurare che la fase acquosa superiore a pH 10.</li>
		<li>Combinare le soluzioni acquose nel passaggio precedente e trasferirli in un imbuto separatore da 500 mL.</li>
		<li>Aggiungere 90 mL di 10% H 2 così 4 soluzione e 50 mL di etere etilico, agitare vigorosamente e separare la fase organica; quindi estrarre la fase acquosa con 30 mL di etere etilico per tre volte (30 mL × 3).</li>
		<li>Combinare le soluzioni di etere etilico nel passaggio 1.2.6 e trasferirli in un altro imbuto separatore da 500 mL.</li>
		<li>Lavarlo con 100 mL di soluzioni sature di NaCl quattro volte (100 mL × 4).</li>
		<li>Aggiungere 4G di anidro MgSO 4 per rimuovere l'eventuale acqua solubile. Filtrare per rimuovere il solido e raccogliere il liquido in un pallone a sfondo sferico uno-collo pulito 250ml.</li>
		<li>Eliminare l'etere etilico con l'evaporatore rotante per ottenere 17,92 g del prodotto grezzo.</li>
	</ol></li></ol> 2. Purificazione di Mono-(2,3-dimethylbutyl) Acido fosfinico <ol><li>preparazione della soluzione di amantadina <ol><li>sciogliere 22,28 g di cloridrato di amantadina in 100 mL di acqua deionizzata in un becher da mL 500.</li>
		<li>Aggiungere 100 mL di soluzione di NaOH, saturi e mescolare per 5 min</li>
		<li>Aggiungere 150 mL di etere etilico e mescolare fino a quando scomparirà il precipitato bianco generato nel passaggio 2.1.2.</li>
		<li>Trasferire le soluzioni in un imbuto separatore da 500 mL, lavare il becher con etere etilico per tre volte (50 mL × 3) e combinarli nell'imbuto stesso.</li>
		<li>Separare la fase acquosa e lavare la fase organica con soluzioni sature di NaCl cinque volte (100 mL × 5).</li>
		<li>Aggiungere 4G di anidro MgSO 4 per rimuovere l'eventuale acqua solubile. Filtro per ottenere la soluzione di etere etilico amantadina.</li>
	</ol></li> <li>Preparazione di amantadina &#8729; mono-(2,3-dimethylbutyl) sale acido fosfinico <ol><li>drop-wise aggiungere il prodotto acido fosfinico grezzo mono-(2,3-dimethylbutyl) alla soluzione di amantadina. Durante la caduta, aggiungere 150 mL di etere etilico per garantire che può mescolare correttamente.</li>
		<li>Lavare il pallone a sfondo sferico uno-collo contenente il mono-(2,3-dimethylbutyl) prodotto acido fosfinico con 50 mL di etere etilico per garantire che tutto il prodotto viene trasferito alla soluzione di amantadina. Sotto agitazione per 30 minuti e lasciate riposare una notte.</li>
		<li>Filtro sotto pressione ridotta e lavare il panello con 200 mL di etere etilico.</li>
	</ol></li> <li>Rilasciare l'acido fosfinico mono-(2,3-dimethylbutyl) <ol><li>trasferire la torta filtrata in un becher da 500 mL, aggiungere 80 mL di 1 M HCl e mescolare per 5 min.</li>
		<li>Aggiungere 70 mL di acetato di etile e mescolare per un altro 5 min</li>
		<li>Trasferire le soluzioni in un imbuto separatore da 250 mL e separare la fase acquosa.</li>
		<li>Estrarre nuovamente la fase acquosa con 40 mL di acetato di etile e combinare le soluzioni di acetato di etile.</li>
		<li>Lavare la soluzione di acetato di etile con 30 mL di 1 M HCl due volte (30 mL × 2) e satura di NaCl tre volte (80 mL × 3), in modo sequenziale.</li>
		<li>Aggiungere 4G anidro MgSO 4 per rimuovere l'eventuale acqua solubile. Filtrare e raccogliere il liquido in un pallone a sfondo sferico uno-collo 250ml.</li>
		<li>Rimuovere l'acetato di etile utilizzando l'evaporatore rotante e ottenere 12,45 g dell'acido fosfinico puro mono-(2,3-dimethylbutyl) (resa: 82,9%).</li>
	</ol></li></ol> 3. Sintesi di (2,3-dimethylbutyl) (2.4.4 &#39;-trimethylpentyl) Acido fosfinico <ol><li>reazione <ol><li>trasferimento tutti del pura mono-(2,3-dimethylbutyl) prodotto acido fosfinico in un 100 mL in acciaio inox rivestito in Teflon autoclave, aggiungere 4,95 g di acido acetico, 25,39 g di diisobutylene, 0,30 g di DTBP, mettere un agitatore magnetico in autoclave e seal it.</li>
		<li>Mettere l'autoclave in un forno tubolare verticale sotto il quale è un mescolatore magnetico e avviare il mescolatore magnetico.</li>
		<li>Impostare il programma di riscaldamento del termoregolatore: riscaldare da temperatura ambiente fino a 135 ° C durante 90 min, mantenere a 135 ° C per 8 h, poi raffreddare a temperatura ambiente, naturalmente. Avviare il programma di riscaldamento.</li>
		<li>Quando il sistema di reazione si raffredda a temperatura ambiente, aggiungere un altro 0,30 g di DTBP e riavviare il programma di riscaldamento.</li>
		<li>Ripetere una volta il punto 3.1.4.</li>
	</ol></li> <li>Post-trattamento <ol><li>diluire il prodotto con 100 mL di etere etilico e poi il trasferimento a un imbuto separatore da 250 mL.</li>
		<li>Lavare con 30 mL di 4% NaOH tre volte (30 mL × 3) per verificare che la fase acquosa superiore a pH 10.</li>
		<li>Aggiungere 70 mL di 10% H 2 così 4 soluzione di acidificare il prodotto.</li>
		<li>Lavare con soluzione satura di NaCl parecchie volte (80 mL ciascuno) fino a quando il pH della fase acquosa è uguale a pH 6-7.</li>
		<li>Aggiungere 4G di anidro MgSO 4 per rimuovere l'eventuale acqua solubile. Filtrare per rimuovere il solido e raccogliere il liquido in un pallone a sfondo sferico uno-collo pulito 250ml.</li>
		<li>Rimuovere l'etere etilico e olefine non reagite con l'evaporatore rotante per ottenere 15,10 g di prodotto grezzo.</li>
	</ol></li></ol> 4. Purificazione di (2,3-dimethylbutyl) (2.4.4 &#39;-trimethylpentyl) Acido fosfinico <ol><li>ottenere co-(2,3-dimethylbutyl) puro (2.4.4 &#39;-trimethylpentyl) complesso acido fosfinico <ol><li>2.30 sciogliere g di NaOH in 40 mL acqua deionizzata. Aggiungere la soluzione di NaOH il matraccio contenente il greggio (2,3-dimethylbutyl) (2.4.4 &#39;-trimethylpentyl) prodotto acido fosfinico e scuoterlo energicamente per 5 min.</li>
		<li>Aggiungi 0,5 M CoCl 2 soluzione goccia a goccia mentre si stringono fino a quando non più precipitato blu viene generato e la soluzione in un matraccio è rosa. < / li> <li>Filtro e lavare il precipitato blu con acqua deionizzata fino a quando la torta del filtro è incolore.</li>
		<li>Trasferire la torta del filtro in un becher da 250 mL, aggiungere 100 mL di acetone, sigillare con pellicola conservante e poi in frigorifero a 4 ° C per una notte.</li>
		<li>Pulverize il precipitato blu di rilasciare eventuali impurità intrappolato nel bulk.</li>
		<li>Filtro e lavarlo con 100 mL di acetone fresco. Asciugare la torta del filtro a temperatura ambiente e poi trasferirlo in un imbuto separatore da 250 mL.</li>
	</ol></li> <li>Rigenerare il (2,3-dimethylbutyl) (2.4.4 &#39;-trimethylpentyl) Acido fosfinico <ol><li>aggiungere 120 mL etere etilico e 80 mL 10% H 2 così 4 e agitare vigorosamente fino a quando il precipitato blu scompare.</li>
		<li>Separare la fase acquosa, lavare l'organico fase in sequenza con 30 mL di 10% H 2 SO 4 una volta e satura NaCl soluzioni diverse volte (80 mL ciascuno) fino a quando il pH della fase acquosa è uguale a pH 6-7.</li>
		<li>Aggiungere 4G di anidro MgSO 4 per rimuovere l'eventuale acqua solubile. Filtro per rimuovere il solido e raccogliere il liquido in un pallone a sfondo sferico uno-collo pulito 250ml.</li>
		<li>Eliminare l'etere etilico utilizzando l'evaporatore rotante e ottenere 11,46 g del prodotto puro (resa: 52,8%).</li>
	</ol>
	</li>
</ol>

<ol>
	<li>Swain, B., Otu, E. O. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Competitive+extraction+of+lanthanides+by+solvent+extraction+using+Cyanex+272:+Analysis,+classification+and+mechanism.">Competitive extraction of lanthanides by solvent extraction using Cyanex 272: Analysis, classification and mechanism.</a> Sep Purif Technol. 83, 82-90 (2011).</li><li>Wang, Y. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+novel+extraction+process+based+on+CYANEX+(R)+572+for+separating+heavy+rare+earths+from+ion-adsorbed+deposit.">The novel extraction process based on CYANEX (R) 572 for separating heavy rare earths from ion-adsorbed deposit.</a> Sep Purif Technol. 151, 303-308 (2015).</li><li>Regel-Rosocka, M., Staszak, K., Wieszczycka, K., Masalska, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Removal+of+cobalt(II)+and+zinc(II)+from+sulphate+solutions+by+means+of+extraction+with+sodium+bis(2,4,4-trimethylpentyl)phosphinate+(Na-Cyanex+272).">Removal of cobalt(II) and zinc(II) from sulphate solutions by means of extraction with sodium bis(2,4,4-trimethylpentyl)phosphinate (Na-Cyanex 272).</a> Clean Technol Envir. 18 (6), 1961-1970 (2016).</li><li>Hereijgers, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Separation+of+Co(II)/Ni(II)+with+Cyanex+272+using+a+flat+membrane+microcontactor:+Stripping+kinetics+study,+upscaling+and+continuous+operation.">Separation of Co(II)/Ni(II) with Cyanex 272 using a flat membrane microcontactor: Stripping kinetics study, upscaling and continuous operation.</a> Chem Eng Res Des. 111, 305-315 (2016).</li><li>Lee, M. S., Banda, R., Min, S. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Separation+of+Hf(IV)-Zr(IV)+in+H2SO4+solutions+using+solvent+extraction+with+D2EHPA+or+Cyanex+272+at+different+reagent+and+metal+ion+concentrations.">Separation of Hf(IV)-Zr(IV) in H2SO4 solutions using solvent extraction with D2EHPA or Cyanex 272 at different reagent and metal ion concentrations.</a> Hydrometallurgy. 152, 84-90 (2015).</li><li>Noori, M., Rashchi, F., Babakhani, A., Vahidi, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Selective+recovery+and+separation+of+nickel+and+vanadium+in+sulfate+media+using+mixtures+of+D2EHPA+and+Cyanex+272.">Selective recovery and separation of nickel and vanadium in sulfate media using mixtures of D2EHPA and Cyanex 272.</a> Sep Purif Technol. 136, 265-273 (2014).</li><li>Li, X. B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermodynamics+and+mechanism+of+vanadium(IV)+extraction+from+sulphate+medium+with+D2EHPA,+EHEHPA+and+CYANEX+272+in+kerosene.">Thermodynamics and mechanism of vanadium(IV) extraction from sulphate medium with D2EHPA, EHEHPA and CYANEX 272 in kerosene.</a> Trans Nonferrous Met Soc China. 22 (2), 461-466 (2012).</li><li>Das, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+the+nature+of+organophosphorous+acid+moiety+on+co-extraction+of+U(VI)+and+mineral+acid+from+aqueous+solutions+using+D2EHPA,+PC88A+and+Cyanex+272.">Effect of the nature of organophosphorous acid moiety on co-extraction of U(VI) and mineral acid from aqueous solutions using D2EHPA, PC88A and Cyanex 272.</a> Hydrometallurgy. 152, 129-138 (2015).</li><li>Baba, A. A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Extraction+of+copper+from+leach+liquor+of+metallic+component+in+discarded+cell+phone+by+Cyanex+(R)+272.">Extraction of copper from leach liquor of metallic component in discarded cell phone by Cyanex (R) 272.</a> JESTEC. 11 (6), 861-871 (2016).</li><li>Du, R. B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microwave-assisted+synthesis+of+dialkylphosphinic+acids+and+a+structure-reactivity+study+in+rare+earth+metal+extraction.">Microwave-assisted synthesis of dialkylphosphinic acids and a structure-reactivity study in rare earth metal extraction.</a> RSC Adv. 5 (126), 104258-104262 (2015).</li><li>Du, R. B., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=alpha,+beta-Substituent+effect+of+dialkylphosphinic+acids+on+anthanide+extraction.">alpha, beta-Substituent effect of dialkylphosphinic acids on anthanide extraction.</a> RSC Adv. 6 (61), 56004-56008 (2016).</li><li>Wang, J. L., Xu, S. X., Li, L. Y., Li, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+organic+phosphinic+acids+and+studies+on+the+relationship+between+their+structure+and+extraction-separation+performance+of+heavy+rare+earths+from+HNO3+solutions.">Synthesis of organic phosphinic acids and studies on the relationship between their structure and extraction-separation performance of heavy rare earths from HNO3 solutions.</a> Hydrometallurgy. 137, 108-114 (2013).</li><li>Hino, A., Nishihama, S., Hirai, T., Komasawa, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Practical+study+of+liquid-liquid+extraction+process+for+separation+of+rare+earth+elements+with+bis+(2-ethylhexyl)+phosphinic+acid.">Practical study of liquid-liquid extraction process for separation of rare earth elements with bis (2-ethylhexyl) phosphinic acid.</a> J Chem Eng Jpn. 30 (6), 1040-1046 (1997).</li><li>Ju, Z. J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+extraction+performance+of+di-decylphosphinic+acid.">Synthesis and extraction performance of di-decylphosphinic acid.</a> Chin J Nonferrous Met. 20 (11), 2254-2259 (2010).</li><li>Li, L. Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dialkyl+phosphinic+acids:+Synthesis+and+applications+as+extractant+for+nickel+and+cobalt+separation.">Dialkyl phosphinic acids: Synthesis and applications as extractant for nickel and cobalt separation.</a> Trans Nonferrous Met Soc China. 20, 205-210 (2010).</li><li>Wang, J. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solvent+extraction+of+rare+earth+ions+from+nitrate+media+with+new+extractant+di-(2,3-dimethylbutyl)-phosphinic+acid.">Solvent extraction of rare earth ions from nitrate media with new extractant di-(2,3-dimethylbutyl)-phosphinic acid.</a> J Rare Earths. 34 (7), 724-730 (2016).</li><li>Hu, W. X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+properties+of+di-tertiary+alkylphosphinic+acids.">Synthesis and properties of di-tertiary alkylphosphinic acids.</a> Chem J Chin Univ-Chin. 15 (6), 849-853 (1994).</li><li>Wang, J. L., Chen, G., Xu, S. M., Li, L. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+of+novel+nonsymmetric+dialkylphosphinic+acid+extractants+and+studies+on+their+extraction-separation+performance+for+heavy+rare+earths.">Synthesis of novel nonsymmetric dialkylphosphinic acid extractants and studies on their extraction-separation performance for heavy rare earths.</a> Hydrometallurgy. 154, 129-136 (2015).</li><li>Wang, J. L., Xie, M. Y., Wang, H. J., Xu, S. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Solvent+extraction+and+separation+of+heavy+rare+earths+from+chloride+media+using+nonsymmetric+(2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic+acid.">Solvent extraction and separation of heavy rare earths from chloride media using nonsymmetric (2,3-dimethylbutyl)(2,4,4'-trimethylpentyl)phosphinic acid.</a> Hydrometallurgy. 167, 39-47 (2017).</li><li>Menoyo, B., Elizalde, M. P., Almela, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Determination+of+the+degradation+compounds+formed+by+the+oxidation+of+thiophosphinic+acids+and+phosphine+sulfides+with+nitric+acid.">Determination of the degradation compounds formed by the oxidation of thiophosphinic acids and phosphine sulfides with nitric acid.</a> Anal Sci. 18 (7), 799-804 (2002).</li><li>Darvishi, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synergistic+effect+of+Cyanex+272+and+Cyanex+302+on+separation+of+cobalt+and+nickel+by+D2EHPA.">Synergistic effect of Cyanex 272 and Cyanex 302 on separation of cobalt and nickel by D2EHPA.</a> Hydrometallurgy. 77, 227-238 (2005).</li></ol>

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Il punto più critico all'interno del protocollo è la sintesi mono-alkylphosphinic acido (Figura 1a). In questa reazione, un rendimento più elevato e meno sottoprodotto di acido dialkylphosphinic è meglio. Aumentando il rapporto molare di NaH2PO2/olefin A migliorerà il rendimento e inibire la generazione di sottoprodotto acido dialkylphosphinic. Tuttavia, un dosaggio elevato di NaH2PO2 sarà anche aumentare il costo e causare u...

Acidi solventi organofosforici sono ampiamente usati nel campo tradizionale Idrometallurgia per estrazione e separazione delle terre rare ioni1,2, metalli non ferrosi (come Co/Ni3,4), metalli rari ( ad esempio Hf/Zr5, V6,7), attinidi8, ecc. Negli ultimi anni, hanno anche attirato più attenzione nei campi della risorsa secondaria riciclaggio e smaltimento dei rifiuti liquidi ad alto livello9. Di-(2-etilesile) (D2EHPA o P204), 2-ethylhexylphosphoric acid mono-2-etilesil estere dell'acido fosforico (EHEHPA, PC 88A o P507) e Di-(2,4, 4'-trimethylpentyl)-Acido fosfinico (Cyanex272), che sono rappresentanti di acidi dialkylphosphoric, alchilfosforici acido mono-alchil esteri e acidi dialkylphosphinic rispettivamente, sono i solventi più comunemente usati. Loro acidità diminuisce nella seguente sequenza: P204 &#62; P507 &#62; Cyanex 272. La corrispondente capacità di estrazione, capacità di estrazione e stripping acidità sono tutti in ordine P204 &#62; P507 &#62; Cyanex 272 e le prestazioni di separazione è nell'ordine opposto. Questi tre solventi sono efficaci nella maggior parte dei casi. Tuttavia, ci sono ancora alcune condizioni dove non sono così efficienti: nella separazione di terre rare pesanti, di cui i principali problemi esistenti sono la scarsa selettività ed elevata acidità stripping per P204 e P507, bassa capacità di estrazione e tendenza di emulsione durante l'estrazione per Cyanex 272. Così, lo sviluppo di nuovi solventi ha attirato maggiore attenzione negli ultimi anni.
La classe di solventi acidi dialkylphosphinic è considerata uno degli aspetti più importanti di ricerca per sviluppare nuovi solventi. Recenti ricerche hanno dimostrato che la capacità di estrazione di acidi dialkylphosphinic dipende in gran parte dalla struttura del alchile sostituenti10,11. Può essere una vasta gamma da significativamente superiore a quello di P507 inferiore a quella di Cyanex 27212. Tuttavia, l'esplorazione di solventi acidi dialkylphosphinic romanzo è limitato per le olefine commerciale struttura10,12,13,14,15, 16. Anche se dialkylphosphinic acidi solventi possono anche essere sintetizzato dal metodo reazione di Grignard, le condizioni di reazione sono rigorosi12,17.
NSDAPA, di cui i due alchili sono diversi, si apre una porta all'esplorazione di nuovi solventi. Rende le strutture di dialkylphosphinic acido più diversificata e sua estrazione e separazione delle prestazioni possono essere ottimizzata modificando sia delle sue strutture di alchile. Il tradizionale metodo sintetico di NSDAPA usato PH3 come una fonte di fosforo, che ha molti svantaggi come alta tossicità, condizioni di reazione rigorosa e difficile purificazione. Recentemente abbiamo segnalato un nuovo metodo per sintetizzare usando ipofosfito di sodio come un fosforo origine (vedere Figura 1) e sintetizzato con successo tre NSDAPAs18NSDAPA. Questo protocollo dettagliato può aiutare nuovi praticanti ripetere gli esperimenti e padroneggiare il metodo sintetico di solventi NSDAPA. Prendiamo (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico come un esempio. I nomi e le strutture di olefine A, l'acido mono-alkylphosphinic intermedio, olefine B e la corrispondente NSDAPA sono riportati nella tabella 1.

<table style="border-collapse:collapse;width:687pt" width="916">
	<colgroup>
		<col style="width:185pt" width="247" />
		<col style="width:290pt" width="387" />
		<col style="width:93pt" width="124" />
		<col style="width:119pt" width="158" />
	</colgroup>
	<tbody>
		<tr height="102" style="height:76.5pt">
			<td class="xl17" height="102" style="width:185pt;height:76.5pt" width="247">sodium hypophosphite hydrate</td>
			<td class="xl17" style="width:290pt" width="387">Tianjin Fuchen Chemical Reagents Factory</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: NaH2PO2&#8729;H2O, purity &#8805;99.0%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">2,3-dimethyl-1-butene</td>
			<td class="xl17" style="width:290pt" width="387">Adamas Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C6H12, purity &#8805;99%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">diisobutylene</td>
			<td class="xl17" style="width:290pt" width="387">Shanghai&#160;Aladdin&#160;Bio-Chem&#160;Technology&#160;Co.,&#160;LTD</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C8H16, purity 97%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">acetic acid</td>
			<td class="xl17" style="width:290pt" width="387">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C2H4O2, purity &#8805;99.5%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">di-tert-butylnperoxide</td>
			<td class="xl17" style="width:290pt" width="387">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C8H18O2, purity &#8805;97.0%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">tetrahydrofuran</td>
			<td class="xl17" style="width:290pt" width="387">Beijing Chemical Works</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C4H8O, purity A.R.</td>
		</tr>
		<tr height="102" style="height:76.5pt">
			<td class="xl17" height="102" style="width:185pt;height:76.5pt" width="247">amantadine hydrochloride</td>
			<td class="xl17" style="width:290pt" width="387">Shanghai&#160;Aladdin&#160;Bio-Chem&#160;Technology&#160;Co.,&#160;LTD</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C10H17N&#8729;HCl, purity 99%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">ethyl ether</td>
			<td class="xl17" style="width:290pt" width="387">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C4H10O, purity &#8805;99.7%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">ethyl acetate</td>
			<td class="xl17" style="width:290pt" width="387">Xilong Chemical Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C4H8O2, purity &#8805;99.5%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">acetone</td>
			<td class="xl17" style="width:290pt" width="387">Beijing Chemical Works</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: C3H6O, purity &#8805;99.5%</td>
		</tr>
		<tr height="75" style="height:56.25pt">
			<td class="xl17" height="75" style="width:185pt;height:56.25pt" width="247">sodium hydroxide</td>
			<td class="xl17" style="width:290pt" width="387">Xilong Chemical Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: NaOH, purity &#8805;96.0%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">concentrated sulfuric acid</td>
			<td class="xl17" style="width:290pt" width="387">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: H2SO4, purity 95-98%</td>
		</tr>
		<tr height="75" style="height:56.25pt">
			<td class="xl17" height="75" style="width:185pt;height:56.25pt" width="247">hydrochloric acid</td>
			<td class="xl17" style="width:290pt" width="387">Beijing Chemical Works</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: HCl, purity 36-38%</td>
		</tr>
		<tr height="75" style="height:56.25pt">
			<td class="xl17" height="75" style="width:185pt;height:56.25pt" width="247">sodium chloride</td>
			<td class="xl17" style="width:290pt" width="387">Sinopharm Chemical Reagent Co., Ltd.</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: NaCl, purity &#8805;99.5%</td>
		</tr>
		<tr height="77" style="height:57.75pt">
			<td class="xl17" height="77" style="width:185pt;height:57.75pt" width="247">anhydrous magnesium sulfate</td>
			<td class="xl17" style="width:290pt" width="387">Tianjin Jinke Institute of Fine Chemical Industry</td>
			<td class="xl17" style="width:93pt" width="124"></td>
			<td class="xl17" style="width:119pt" width="158">Molecular formula: MgSO4, purity &#8805;99.0%</td>
		</tr>
		<tr height="103" style="height:77.25pt">
			<td class="xl19" height="103" style="width:185pt;height:77.25pt" width="247">Cobalt(II) chloride hexahydrate</td>
			<td class="xl19" style="width:290pt" width="387">Xilong Chemical Co., Ltd.</td>
			<td class="xl19" style="width:93pt" width="124"></td>
			<td class="xl19" style="width:119pt" width="158">Molecular formula: CoCl2&#8729;6H2O, purity &#8805;99.0%</td>
		</tr>
	</tbody>
</table>

synthesis of high purity nonsymmetric dialkylphosphinic acid extractants

Vi presentiamo la sintesi di (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico come esempio per illustrare un metodo per la sintesi di elevata purezza il dialkylphosphinic acido solventi. Ipofosfito di sodio basso tossico è stato scelto come la fonte di fosforo a reagire con olefine un (2,3-dimetil-1-butene) per generare un acido monoalkylphosphinic intermedio. L'amantadina è stata adottata per rimuovere il sottoprodotto di acido dialkylphosphinic, come solo l'acido monoalkylphosphinic può reagire con amantadina per formare un sale acido di amantadine∙mono-alkylphosphinic, mentre l'acido dialkylphosphinic non può reagire con amantadina a causa sua grande impedimento sterico. L'acido purificato monoalkylphosphinic quindi è stato reagito con olefine B (diisobutylene) per produrre il dialkylphosphinic acido (NSDAPA). L'acido non reagito monoalkylphosphinic possa essere facilmente rimossi con un semplice post-trattamento base-acido e altre impurità organiche possono essere separati attraverso la precipitazione del sale di cobalto. La struttura della (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico è stata confermata dalla RMN 31P, 1H NMR, ESI-MS e FT-IR. La purezza è stata determinata con un metodo di titolazione potenziometrica, ed i risultati indicano che la purezza può superare i 96%.

31 Gli spettri RMN P sono stati raccolti per l'acido fosfinico mono-(2,3-dimethylbutyl) prima e dopo la purificazione dal metodo amantadina (Figura 1a-b). 31 Gli spettri RMN P, spettri di 1H NMR, MS spettri e spettri FT-IR sono stati raccolti per (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico (vedere Figura 3, Figura 4, <strong class="x...

Watch this Scientific Journal Video about Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants at JoVE.com

Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants

Sintesi di elevata purezza il Dialkylphosphinic acido solventi

Un protocollo per la sintesi di elevata purezza il dialkylphosphinic acido solventi è presentato, prendendo (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico come un esempio.

We present the synthesis of (2,3-dimethylbutyl)(2,4,4&#39;-trimethylpentyl)phosphinic acid as an example to demonstrate a method for the synthesis of high ...

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7.4K Views.  University of Science and Technology Beijing. Un protocollo per la sintesi di elevata purezza il dialkylphosphinic acido solventi è presentato, prendendo (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) Acido fosfinico come un esempio.

Video: Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants

Synthesis of Antiviral Tetrahydrocarbazole Derivatives by Photochemical and Acid-catalyzed C-H Functionalization via Intermediate Peroxides (CHIPS)

The direct functionalization of C-H bonds is an important and long standing goal in organic chemistry. Such transformations can be very powerful in order to streamline synthesis by saving steps, time and material compared to conventional methods that require the introduction and removal of activating or directing groups. Therefore, the functionalization of C-H bonds is also attractive for green chemistry. Under oxidative conditions, two C-H bonds or one C-H and one heteroatom-H bond can be transformed to C-C and C-heteroatom bonds, respectively. Often these oxidative coupling reactions require synthetic oxidants, expensive catalysts or high temperatures. Here, we describe a two-step procedure to functionalize indole derivatives, more specifically tetrahydrocarbazoles, by C-H amination using only elemental oxygen as oxidant. The reaction uses the principle of C-H functionalization via Intermediate PeroxideS (CHIPS). In the first step, a hydroperoxide is generated oxidatively using visible light, a photosensitizer and elemental oxygen. In the second step, the N-nucleophile, an aniline, is introduced by Br&#248;nsted-acid catalyzed activation of the hydroperoxide leaving group. The products of the first and second step often precipitate and can be conveniently filtered off. The synthesis of a biologically active compound is shown.

Synthesis of Antiviral Tetrahydrocarbazole Derivatives by Photochemical and Acid-catalyzed C-H Functionalization via Intermediate Peroxides CHIPS

A two-step procedure for the synthesis of pharmaceutically active indole-derivatives by C-H functionalization with anilines is described, using photo- and Br&#248;nsted acid catalysis.

Sintesi di derivati ​​antivirale Tetrahydrocarbazole da fotochimica e acido-catalizzata CH funzionalizzazione via intermedi perossidi (CHIPS)

The direct functionalization of C-H bonds is an important and long standing goal in organic chemistry. Such transformations can be very powerful in order ...

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Synthesis of Immunotargeted Magneto-plasmonic Nanoclusters

Magnetic and plasmonic properties combined in a single nanoparticle provide a synergy that is advantageous in a number of biomedical applications including contrast enhancement in novel magnetomotive imaging modalities, simultaneous capture&#160;and detection of circulating tumor cells (CTCs),&#160;and multimodal molecular imaging combined with photothermal therapy of cancer cells. These applications have stimulated significant interest in development of protocols for synthesis of magneto-plasmonic nanoparticles with optical absorbance in the near-infrared (NIR) region and a strong magnetic moment. Here, we present a novel protocol for synthesis of such hybrid nanoparticles that is based on an oil-in-water microemulsion method. The unique feature of the protocol described herein is synthesis of magneto-plasmonic nanoparticles of various sizes from primary blocks which also have magneto-plasmonic characteristics. This approach yields nanoparticles with a high density of magnetic and plasmonic functionalities which are uniformly distributed throughout the nanoparticle volume. The hybrid nanoparticles can be easily functionalized by attaching antibodies through the Fc moiety leaving the Fab portion that is responsible for antigen binding available for targeting.

Here, we describe a protocol for synthesis of magneto-plasmonic nanoparticles with a strong magnetic moment and a strong near-infrared (NIR) absorbance. The protocol also includes antibody conjugation to the nanoparticles through the Fc moiety for various biomedical applications which require molecular specific targeting.

Sintesi di Immunotargeted magneto-plasmonica nanocluster

Magnetic and plasmonic properties combined in a single nanoparticle provide a synergy that is advantageous in a number of biomedical applications ...

Synthesis of Indoxyl-glycosides for Detection of Glycosidase Activities

Indoxyl glycosides proved to be valuable and versatile tools for monitoring glycosidase activities. Indoxyls are released by enzymatic hydrolysis and are rapidly oxidized, for example by atmospheric oxygen, to indigo type dyes. This reaction enables fast and easy screening in vivo without isolation or purification of enzymes, as well as rapid tests on agar plates or in solution (e.g., blue-white screening, micro-wells) and is used in biochemistry, histochemistry, bacteriology and molecular biology. Unfortunately the synthesis of such substrates proved to be difficult, due to various side reactions and the low reactivity of the indoxyl hydroxyl function. Especially for glucose type structures low yields were observed. Our novel approach employs indoxylic acid ester as key intermediates. Indoxylic acid esters with varied substitution patterns were prepared on scalable pathways. Phase transfer glycosylations with those acceptors and peracetylated glycosyl halides can be performed under common conditions in high yields. Ester cleavage and subsequent mild silver mediated glycosylation yields the peracetylated indoxyl glycosides in high yields. Finally deprotection is performed according to Zempl&#233;n.

Indoxyl glycosides are well-established and widely used tools for enzyme screening and enzyme activity monitoring. Especially for glucose type structures previous syntheses proved to be challenging and low yielding. Our novel approach employs indoxylic acid esters as precious intermediates to yield a considerable number of indoxyl glycosides in good yields.

Sintesi di indoxyl-glicosidi per il rilevamento di glicosidasi Attività

Indoxyl glycosides proved to be valuable and versatile tools for monitoring glycosidase activities. Indoxyls are released by enzymatic hydrolysis and are ...

Synthesis and Characterization of Supramolecular Colloids

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical properties for applications in photonics, drug delivery and coating technology. Here we present a new family of colloidal building blocks, coined supramolecular colloids, whose self-assembly is controlled through surface-functionalization with a benzene-1,3,5-tricarboxamide (BTA) derived supramolecular moiety. Such BTAs interact via directional, strong, yet reversible hydrogen-bonds with other identical BTAs. Herein, a protocol is presented that describes how to couple these BTAs to colloids and how to quantify the number of coupling sites, which determines the multivalency of the supramolecular colloids. Light scattering measurements show that the refractive index of the colloids is almost matched with that of the solvent, which strongly reduces the van der Waals forces between the colloids. Before photo-activation, the colloids remain well dispersed, as the BTAs are equipped with a photo-labile group that blocks the formation of hydrogen-bonds. Controlled deprotection with UV-light activates the short-range hydrogen-bonds between the BTAs, which triggers the colloidal self-assembly. The evolution from the dispersed state to the clustered state is monitored by confocal microscopy. These results are further quantified by image analysis with simple routines using ImageJ and Matlab. This merger of supramolecular chemistry and colloidal science offers a direct route towards light- and thermo-responsive colloidal assembly encoded in the surface-grafted monolayer.

A protocol for the synthesis and characterization of colloids coated with supramolecular moieties is described. These supramolecular colloids undergo self-assembly upon the activation of the hydrogen-bonds between the surface-anchored molecules by UV-light.

Sintesi e caratterizzazione di supramolecolari colloidi

Control over colloidal assembly is of utmost importance for the development of functional colloidal materials with tailored structural and mechanical ...

Hydroquinone Based Synthesis of Gold Nanorods

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the synthetic methods for the preparation of gold nanorods are still not fully optimized. In this paper we describe a new, highly efficient, two-step protocol based on the use of hydroquinone as a mild reducing agent. Our approach allows the preparation of nanorods with a good control of size and aspect ratio (AR) simply by varying the amount of hexadecyl trimethylammonium bromide (CTAB) and silver ions (Ag+) present in the "growth solution". By using this method, it is possible to markedly reduce the amount of CTAB, an expensive and cytotoxic reagent, necessary to obtain the elongated shape. Gold nanorods with an aspect ratio of about 3 can be obtained in the presence of just 50 mM of CTAB (versus 100 mM used in the standard protocol based on the use of ascorbic acid), while shorter gold nanorods are obtained using a concentration as low as 10 mM.

This paper describes a protocol for the synthesis of gold nanorods, based on the use of hydroquinone as reducing agent, plus the different mechanisms for controlling their size and aspect ratio.

Idrochinone Based Sintesi di oro Nanorods

Gold nanorods are an important kind of nanoparticles characterized by peculiar plasmonic properties. Despite their widespread use in nanotechnology, the ...

Synthesis of Hierarchical ZnO/CdSSe Heterostructure Nanotrees

A two-step chemical vapor deposition procedure is here employed to prepare tree-like hierarchical ZnO/CdSSe hetero-nanostructures. The structures are composed of CdSSe branches grown on ZnO nanowires that are vertically aligned on a transparent sapphire substrate. The morphology was measured via scanning electron microscopy. The crystal structure was determined by X-ray powder diffraction analysis. Both the ZnO stem and CdSSe branches have a predominantly wurtzite crystal structure. The mole ratio of S and Se in the CdSSe branches was measured by energy dispersive X-ray spectroscopy. The CdSSe branches result in strong visible light absorption. Photoluminescence (PL) spectroscopy showed that the stem and branches form a type-II heterojunction. PL lifetime measurements showed a decrease in the lifetime of emission from the trees when compared to emission from individual ZnO stems or CdSSe branches and indicate fast charge transfer between CdSSe and ZnO. The vertically aligned ZnO stems provide a direct electron transport pathway to the substrate and allow for efficient charge separation after photoexcitation by visible light. The combination of the abovementioned properties makes ZnO/CdSSe nanotrees promising candidates for applications in solar cells, photocatalysis, and opto-electronic devices.

Here, we prepare and characterize novel tree-like hierarchical ZnO/CdSSe nanostructures, where CdSSe branches are grown on vertically aligned ZnO nanowires. The resulting nanotrees are a potential material for solar energy conversion and other opto-electronic devices.

Sintesi di Hierarchical ZnO / CdSSe Heterostructure Nanotrees

A two-step chemical vapor deposition procedure is here employed to prepare tree-like hierarchical ZnO/CdSSe hetero-nanostructures. The structures are ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

Modificare il metodo di precipitazione chimica per la sintesi di Nb2O5 catalizzatori di nichel Bulk con elevata superficie specifica

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Synthesis of Substrate-Bound Au Nanowires Via an Active Surface Growth Mechanism

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a challenge, as it requires asymmetric growth of symmetric crystals. Here, we report a distinctive synthesis of substrate-bound Au nanowires. This template-free synthesis employs thiolated ligands and substrate adsorption to achieve the continuous asymmetric deposition of Au in solution at ambient conditions. The thiolated ligand prevented the Au deposition on the exposed surface of the seeds, so the Au deposition only occurs at the interface between the Au seeds and the substrate. The side of the newly deposited Au nanowires is immediately covered with the thiolated ligand, while the bottom facing the substrate remains ligand-free and active for the next round of Au deposition. We further demonstrate that this Au nanowire growth can be induced on various substrates, and different thiolated ligands can be used to regulate the surface chemistry of the nanowires. The diameter of the nanowires can also be controlled with mixed ligands, in which another &#34;bad&#34; ligand could turn on the lateral growth. With the understanding of the mechanism, Au nanowire-based nanostructures can be designed and synthesized.

We report a solution-based method to synthesize substrate-bound Au nanowires. By tuning the molecular ligands used during the synthesis, the Au nanowires can be grown from various substrates with different surface properties. Au nanowire-based nanostructures can also be synthesized by adjusting the reaction parameters.

Sintesi di nanofili Au associato a substrato tramite un meccanismo di crescita superficiale attiva

Advancing synthetic capabilities is important for the development of nanoscience and nanotechnology. The synthesis of nanowires has always been a ...

Solid-phase Synthesis of [4.4] Spirocyclic Oximes

A convenient synthetic route for spirocyclic heterocycles is well sought after due to the molecule&#39;s potential use in biological systems. By means of solid-phase synthesis, regenerating Michael (REM) linker strategies, and 1,3-dipolar cycloaddition, a library of structurally similar heterocycles, both with and without a spirocyclic center, can be constructed. The main advantages of the solid-support synthesis are as follows: first, each reaction step can be driven to completion using a large excess of reagents resulting in high yields; next, the use of commercially available starting materials and reagents keep the costs low; finally, the reaction steps are easy to purify via simple filtration. The REM linker strategy is attractive because of its recyclability and traceless nature. Once a reaction scheme is completed, the linker can be reused multiple times. In a typical solid-phase synthesis, the product contains either a part of or the whole linker, which can prove undesirable. The REM linker is &#34;traceless&#34; and the point of attachment between the product and the polymer is indistinguishable. The high diastereoselectivity of the intramolecular 1,3-dipolar cycloaddition is well documented. Limited by the insolubility of the solid support, the reaction progression can only be monitored by a change in the functional groups (if any) via infrared (IR) spectroscopy. Thus, the structural identification of intermediates cannot be characterized by conventional nuclear magnetic resonance (NMR) spectroscopy. Other limitations to this method stem from the compatibilities of the polymer/linker to the desired chemical reaction scheme. Herein we report a protocol that allows for the convenient production of spirocyclic heterocycles that, with simple modifications, can be automated with high-throughput techniques.

Here we present a protocol to demonstrate an efficient method for the synthesis of spirocyclic heterocycles. The five-step process utilizes solid-phase synthesis and regenerating Michael linker strategies. Generally difficult to synthesize, we present a customizable method for the synthesis of spirocyclic molecules otherwise inaccessible to other modern approaches.

Sintesi in fase solida di [4,4] Spirocyclic ossime

A convenient synthetic route for spirocyclic heterocycles is well sought after due to the molecule&#39;s potential use in biological systems. By means of ...

Synthesis and Characterization of Amphiphilic Gold Nanoparticles

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of their interactions with cell membranes, lipid bilayers, and viruses. The hydrophilic ligands make these particles colloidally stable in aqueous solutions and the combination with hydrophobic ligands creates an amphiphilic particle that can be loaded with hydrophobic drugs, fuse with the lipid membranes, and resist nonspecific protein adsorption. Many of these properties depend on nanoparticle size and the composition of the ligand shell. It is, therefore, crucial to have a reproducible synthetic method and reliable characterization techniques that allow the determination of nanoparticle properties and the ligand shell composition. Here, a one-phase chemical reduction, followed by a thorough purification to synthesize these nanoparticles with diameters below 5 nm, is presented. The ratio between the two ligands on the surface of the nanoparticle can be tuned through their stoichiometric ratio used during synthesis. We demonstrate how various routine techniques, such as transmission electron microscopy (TEM), nuclear magnetic resonance (NMR), thermogravimetric analysis (TGA), and ultraviolet-visible (UV-Vis) spectrometry, are combined to comprehensively characterize the physicochemical parameters of the nanoparticles.

Amphiphilic gold nanoparticles can be used in many biological applications. A protocol to synthesize gold nanoparticles coated by a binary mixture of ligands and a detailed characterization of these particles is presented.

Sintesi e caratterizzazione delle nanoparticelle d'oro dell'anfifile

Gold nanoparticles covered with a mixture of 1-octanethiol (OT) and 11-mercapto-1-undecane sulfonic acid (MUS) have been extensively studied because of ...