Bu eser Ulusal Doğa Bilim Vakfı Çin (21301104), orta üniversiteler (FRF-TP-16-019A3) ve devlet anahtar laboratuvar, Kimya Mühendisliği (SKL-ChE-14A04) için temel araştırma fonu tarafından desteklenmiştir.

1. sentez, Mono-(2,3-dimethylbutyl) phosphinic asit 18 , 19 <ol><li>tepki <ol><li>tartmak 31.80 g sodyum hipofosfit hidrat, 16.00 g Asetik asit, 8,42 g 2,3-Dimetil-1-butene, 0.73 g di - tert-butylnperoxide (DTBP) ve 25.00 g tetrahydrofuran (THF) 100 mL Teflon kaplı paslanmaz çelik basınçlı kap içine bir manyetik karıştırıcı basınçlı kap koymak ve bunu mühür</li>
		<li>Manyetik stirringapparatus altında olan bir dikey tüp ocağında basınçlı kap koymak. Manyetik karıştırma aparatı başlatın ve hızı 800 rpm'de ayarlayın.</li>
		<li>Ayarlamak için otoklav bağlı sıcaklık denetleyicisinin Isıtma programı: ısı oda sıcaklığından 120 ° C-90 dk sırasında 8 h için 120 ° C'de korumak sonra doğal olarak oda sıcaklığına kadar sakin ol. Isıtma programını başlatmak.</li>
	</ol></li> <li>Tedavi sonrası <ol><li>ürünleri bir 250 mL bir boyun yuvarlak alt şişesi aktarmak, Teflon kaplama 50 mL THF ile yıkayın ve tüm ürünler aktarılmasını sağlamak için aynı balonun eklemek.</li>
		<li>Çıkarmak belgili tanımlık THF ve döner Buharlaştırıcı kullanarak unreacted olefins.</li>
		<li>Residua 250 mL huni ayıran içine aktarmak, sırasıyla şişesi 80 mL etil eter ve 30 mL deiyonize su ile yıkayın ve onları tüm ürünler aktarılmasını sağlamak için aynı ayıran huni içine eklemek.</li>
		<li>Ekle 50 mL % 4 NaOH çözüm yukarıdaki ayıran huni içine şiddetle çalkalanır ve sulu faz ayırın. 20 mL % 4 NaOH çözümleri ile organik faz üç kez ayıklamak (20 mL × sulu faz pH 10 aşıyor emin olmak için 3).</li>
		<li>Sulu çözümler yukarıdaki adımda birleştirmek ve huni ayıran 500 mL aktarmak.</li>
		<li>Ekleyin 90 mL % 10 H 2 4 çözüm ve 50 mL etil eter, şiddetle çalkalanır ve organik faz; ayrı sonra özü 30 mL etil eter ile sulu faz üç kez (30 mL × 3).</li>
		<li>Adım 1.2.6 etil eter çözümlerinde birleştirmek ve huni ayıran başka bir 500 mL transfer.</li>
		<li>(100 mL × 4) ile 100 mL doymuş NaCl çözümleri dört yıka.</li>
		<li>Çözünür su kaldırmak için susuz MgSO 4 4 g ekleyin. Katı kaldırmak için filtre ve sıvı temiz 250 mL bir boyun yuvarlak alt kabı içinde toplamak.</li>
		<li>Rotary Evaporatör 17.92 g ham ürün elde etmek için kullanarak etil eter kaldırmak.</li>
	</ol></li></ol> 2. Mono-(2,3-dimethylbutyl) phosphinic asit arıtma <ol><li>Amantadin çözüm hazırlanması <ol><li>bir 500 mL ölçek deiyonize su 100 ml Amantadin hidroklorür 22.28 g geçiyoruz.</li>
		<li>Doymuş NaOH çözüm ve 5 dakika süreyle heyecan eklemek 100 mL</li>
		<li>150 mL etil eter ekleyin ve karıştırın kadar 2.1.2 adımda oluşturulan beyaz çökelti kaybolur.</li>
		<li>Çözümleri huni ayıran 500 mL aktarmak, etil eter ile kabı için üç kez yıkayın (50 mL × 3) ve onları aynı ayıran huni birleştirmek.</li>
		<li>Sulu faz ayırmak ve doymuş NaCl çözümleri beş ile organik faz (100 mL × 5) yıkayın.</li>
		<li>Çözünür su kaldırmak için susuz MgSO 4 4 g ekleyin. Amantadin etil eter çözüm elde etmek için filtre.</li>
	</ol></li> <li>Amantadin hazırlanması &#8729; mono-(2,3-dimethylbutyl) phosphinic asit tuz <ol><li>drop-wise ham mono-(2,3-dimethylbutyl) phosphinic asit ürün Amantadin ekleyin. Bırakma sırasında etil eter düzgün heyecan olabilir emin olmak için 150 mL ekleyin.</li>
		<li>Mono-(2,3-dimethylbutyl) phosphinic asit ürün ile etil eter tüm ürün Amantadin çözüm için transfer edilir emin olmak için 50 mL içeren bir boyun yuvarlak alt şişeye yıka. Stir için 30 dk ve gecede oturup izin.</li>
		<li>Filtre küçük basınç azalır ve 200 mL etil eter filtre pastayla yıkayın.</li>
	</ol></li> <li>Mono-(2,3-dimethylbutyl) phosphinic asit serbest <ol><li>filtre uygulanmış kek 500 mL kabı içine aktarmak, 1 M HCL, 80 mL ekleyin ve karıştırın için 5 dk.</li>
		<li>Eklemek 70 mL Etil asetat ve heyecan başka bir 5 dakika süreyle</li>
		<li>Çözümleri huni ayıran 250 mL aktarmak ve sulu faz ayırın.</li>
		<li>Sulu faz 40 mL Etil asetat ile tekrar ayıklar ve Etil asetat çözümleri birleştirir.</li>
		<li>30 mL (30 mL × 2) 1 M HCL iki kez Etil asetat Çözümle yıkama ve NaCl üç ardışık olarak (80 mL × 3), doymuş.</li>
		<li>Çözünür su kaldırmak için 4 g susuz MgSO 4 ekleyin. Filtre ve sıvı bir 250 mL bir boyun yuvarlak alt şişesi içinde toplamak.</li>
		<li>Etil asetat rotary Evaporatör kullanarak kaldırın ve 12.45 g saf mono-(2,3-dimethylbutyl) phosphinic asit elde etmek (verim: %82.9).</li>
	</ol></li></ol> 3. Sentezi (2,3-dimethylbutyl) (2,4,4 &#39;-trimethylpentyl) phosphinic asit <ol><li>tepki <ol><li>Transfer tüm saf mono-(2,3-dimethylbutyl) phosphinic asit ürünün içine 100 mL Teflon kaplı paslanmaz çelik Otoklav, Asetik asit, diisobutylene, DTBP, 0.30 g 25.39 g 4.95 g ekleyin, bir manyetik karıştırıcı basınçlı kap koymak ve bunu mühür</li>
		<li>Altında olan bir manyetik karıştırma aparatı dikey tüp ocağında basınçlı kap koymak ve manyetik karıştırma aparatı başlar.</li>
		<li>Sıcaklık denetleyicisinin Isıtma program ayarla: ısı oda sıcaklığından 135 ° C-90 dk sırasında 8 h 135 ° C'de korumak sonra doğal olarak oda sıcaklığına kadar sakin ol. Isıtma programını başlatmak.</li>
		<li>Reaksiyon sistemi oda sıcaklığına soğuduğunda DTBP başka bir 0.30 g ekleyin ve Isıtma programı yeniden.</li>
		<li>Tekrarlama adım 3.1.4 bir kez.</li>
	</ol></li> <li>Tedavi sonrası <ol><li>100 mL etil eter ürünüyle sulandırmak ve 250 bir huni ayıran mL transfer.</li>
		<li>30 mL % 4 ile yıkayın NaOH üç kez (30 mL × 3) Bu sulu faz pH 10 aşıyor emin olmak için.</li>
		<li>Kadar % 10 H 2 70 mL ekleyin ürün acidify için 4 çözüm.</li>
		<li>Sulu faz pH pH 6-7 eşittir kadar birkaç kez (80 mL her) ile doymuş NaCl çözüm yıka.</li>
		<li>Çözünür su kaldırmak için susuz MgSO 4 4 g ekleyin. Katı kaldırmak için filtre ve sıvı temiz 250 mL bir boyun yuvarlak alt kabı içinde toplamak.</li>
		<li>Çıkarmak belgili tanımlık etil eter ve döner Buharlaştırıcı 15,10 g ham ürün elde etmek için kullanarak unreacted olefins.</li>
	</ol></li></ol> 4. Arıtma (2,3-dimethylbutyl) (2,4,4 &#39;-trimethylpentyl) phosphinic asit <ol><li>saf co-(2,3-dimethylbutyl) elde etmek (2,4,4 &#39;-trimethylpentyl) phosphinic asit karmaşık <ol><li>erimesi 2,30 g NaOH 40 ml deiyonize su. Ham içeren şişeye NaOH çözüm ekleyin (2,3-dimethylbutyl) (2,4,4 &#39;-trimethylpentyl) phosphinic asit ürün ve şiddetle 5 dk. salla</li>
		<li>Ekle 0,5 M CoCl 2 çözüm daha fazla mavi çökelti oluşturulur ve şişeye çözümde pembe. kadar sallayarak süre dropwise < /li> <li>Filtre ve yıkama filtresi kek kadar deiyonize su ile mavi çökelti renksiz.</li>
		<li>250 mL kabı filtre kek transfer 100 mL aseton ekleyin koruyucu film ile kapatın ve sonra bir gece için 4 ° C'de soğutmak.</li>
		<li>Herhangi bir yabancı maddelerin serbest bırakmak için mavi çökelti tuzağa toplu olarak Pulverize.</li>
		<li>Filtre ve 100 mL taze aseton ile yıkayın. Oda sıcaklığında filtre pasta kuru ve sonra huni ayıran 250 mL transfer.</li>
	</ol></li> <li>Yeniden (2,3-dimethylbutyl) (2,4,4 &#39;-trimethylpentyl) phosphinic asit <ol><li>4 ve shake şiddetle kadar mavi çökelti kaybolur 120 mL etil eter ve 80 mL % 10 H 2 ekleyin.</li>
		<li>Sulu faz ayrı, organik yıkama aşama sıralı olarak 30 mL % 10 H 2 SO 4 bir kez ve sulu faz pH pH 6-7 eşittir kadar NaCl çözümler birkaç kez (80 mL her) doymuş.</li>
		<li>Çözünür su kaldırmak için susuz MgSO 4 4 g ekleyin. Katı kaldırma ve sıvı temiz 250 mL bir boyun yuvarlak alt kabı içinde toplamak için filtre.</li>
		<li>Etil eter rotary Evaporatör kullanarak kaldırın ve 11.46 g saf ürün elde etmek (verim: %52,8).</li>
	</ol>
	</li>
</ol>

<ol>
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Yazarlar ifşa gerek yok.

En kritik protokol içinde mono-alkylphosphinic asit sentezi (şekil 1bir) adımdır. Bu tepki, daha yüksek bir verim ve daha az dialkylphosphinic asit yan ürün daha iyi. NaH2PO2/olefin A molar oranı artan verim artırmak ve dialkylphosphinic asit yan ürün üretimi inhibe. Ancak, bir büyük NaH2PO2 doz Ayrıca maliyet artırmak ve coşkulu bir soruna neden. NaH2PO2/olefin A tercih edilen molar oranı 3:...

Asidik organofosfor extractants yaygın olarak geleneksel hydrometallurgy alanında ayıklama ve nadir toprak iyonları1,2, demir harici metaller (Co/Ni3,4gibi) nadir metaller (ayrılması için kullanılır Hf/Zr gibi5V6,7), aktinitleri8, vb. Son yıllarda, onlar da ikincil kaynak geri dönüşüm ve üst düzey sıvı atık bertaraf9alanlarında daha fazla dikkat çekmiştir. Di-(2-ethylhexyl) fosforik asit (D2EHPA veya P204), 2-ethylhexylphosphoric asit mono-2-ethylhexyl ester (EHEHPA, PC 88A veya P507) ve Di-(2,4, 4'-trimethylpentyl)-dialkylphosphoric asit temsilcileri olan phosphinic asit (Cyanex272), Aminobenzensülforik asit mono alkil esterleri ve dialkylphosphinic asit sırasıyla, en sık kullanılan extractants vardır. Onların Asitlik aşağıdaki sırayla azalır: P204 &#62; P507 &#62; Cyanex 272. Karşılık gelen çıkarma yeteneği, ayıklama kapasite ve sıyırma Asitlik sırasına göre tüm P204 vardır &#62; P507 &#62; Cyanex 272 ve ayrılık performans olduğunu ters sırada. Bu üç extractants çoğu zaman etkili olur. Ancak, hala bazı koşullar vardır nereye onlar are değil çok verimli: ağır nadir toprak elementleri ayırma, varolan ana sorunları olan zavallı seçicilik ve P204 ve P507, yüksek sıyırma asit düşük çekme kapasitesi ve emülsiyon eğilim Cyanex 272 için ayıklama sırasında. Böylece, roman extractants gelişimi son yıllarda daha çok dikkat çekti.
Dialkylphosphinic asit extractants sınıf yeni extractants geliştirmek için en önemli araştırma unsurlarından biri olarak kabul edilir. Son araştırmalar çıkarma yeteneği dialkylphosphinic asit alkil organik10,11yapısına büyük ölçüde bağlı olduğunu gösterdi. Bu önemli ölçüde daha yüksek P507 bundan Cyanex 27212daha düşürmek için daha geniş bir aralıktan olabilir. Ancak, roman dialkylphosphinic asit extractants keşfi ticari organik yapısı10,12,13,14,-15sınırlı, 16. Dialkylphosphinic asit extractants da Grignard reaksiyonu yöntemi tarafından sentez rağmen sıkı12,17tepki koşullardır.
NSDAPA, iki alkyls farklı olan yeni extractants keşfi bir kapı açar. Dialkylphosphinic asit yapıları daha farklı hale getirir ve çıkarma ve ayrılık performans onun alkil yapıları her ikisini değiştirerek ince ayar. NSDAPA geleneksel sentetik yöntemi PH3 yüksek toksisite, titiz reaksiyon koşulları ve zor arıtma gibi birçok dezavantajları vardır bir fosfor kaynağı olarak kullanılır. Son zamanlarda bir fosfor (bkz. şekil 1) kaynağı ve başarılı bir şekilde üç NSDAPAs18sentezlenmiş olarak sodyum hipofosfit kullanarak NSDAPA sentez için yeni bir yöntem bildirdi. Bu ayrıntılı Protokolü deneyler yineleyin ve NSDAPA extractants sentetik yöntemi usta yeni uygulayıcıları yardımcı olabilir. Biz almak (2, 3-dimethylbutyl) (2,4, 4'-trimethylpentyl) bir örnek olarak phosphinic asit. Adları ve yapıları olefin A, ara mono-alkylphosphinic asit, organik B ve karşılık gelen NSDAPA, Tablo 1' de görüntülenir.

<table><tbody><tr><td>2,3-dimethyl-1-butene</td><td>Adamas Reagent Co., Ltd.</td><td></td><td>Molecular formula: C&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;6&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;H&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;12&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;, purity &amp;ge;99%&lt;/span&gt;</td></tr><tr><td>diisobutylene</td><td>Shanghai&amp;nbsp;Aladdin&amp;nbsp;Bio-Chem&amp;nbsp;Technology&amp;nbsp;Co.,&amp;nbsp;LTD</td><td></td><td>Molecular formula: C&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;8&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;H&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;16&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;, purity 97%&lt;/span&gt;</td></tr><tr><td>acetic acid</td><td>Sinopharm Chemical Reagent Co., Ltd.</td><td></td><td>Molecular formula: C&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;2&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;H&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;4&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;O&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;2&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;, purity &amp;ge;99.5%&lt;/span&gt;</td></tr><tr><td>di-&lt;span class=&quot;font9&quot;&gt;tert&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;-butylnperoxide&lt;/span&gt;</td><td>Sinopharm Chemical Reagent Co., Ltd.</td><td></td><td>Molecular formula: C&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;8&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;H&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;18&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;O&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;2&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;, purity &amp;ge;97.0%&lt;/span&gt;</td></tr><tr><td>tetrahydrofuran</td><td>Beijing Chemical Works</td><td></td><td>Molecular formula: C&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;4&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;H&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;8&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;O, purity A.R.&lt;/span&gt;</td></tr><tr><td>ethyl ether</td><td>Sinopharm Chemical Reagent Co., Ltd.</td><td></td><td>Molecular formula: C&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;4&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;H&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;10&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;O, purity &amp;ge;99.7%&lt;/span&gt;</td></tr><tr><td>ethyl acetate</td><td>Xilong Chemical Co., Ltd.</td><td></td><td>Molecular formula: C&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;4&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;H&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;8&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;O&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;2&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;, purity &amp;ge;99.5%&lt;/span&gt;</td></tr><tr><td>acetone</td><td>Beijing Chemical Works</td><td></td><td>Molecular formula: C&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;3&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;H&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;6&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;O, purity &amp;ge;99.5%&lt;/span&gt;</td></tr><tr><td>sodium hydroxide</td><td>Xilong Chemical Co., Ltd.</td><td></td><td>Molecular formula: NaOH, purity &amp;ge;96.0%</td></tr><tr><td>concentrated sulfuric acid</td><td>Sinopharm Chemical Reagent Co., Ltd.</td><td></td><td>Molecular formula: H&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;2&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;SO&lt;/span&gt;&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;4&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;, purity 95-98%&lt;/span&gt;</td></tr><tr><td>hydrochloric acid</td><td>Beijing Chemical Works</td><td></td><td>Molecular formula: HCl, purity 36-38%</td></tr><tr><td>sodium chloride</td><td>Sinopharm Chemical Reagent Co., Ltd.</td><td></td><td>Molecular formula: NaCl, purity &amp;ge;99.5%</td></tr><tr><td>anhydrous magnesium sulfate</td><td>Tianjin Jinke Institute of Fine Chemical Industry</td><td></td><td>Molecular formula: MgSO&lt;span class=&quot;font8&quot;&gt;&lt;sub&gt;4&lt;/sub&gt;&lt;/span&gt;&lt;span class=&quot;font7&quot;&gt;, purity &amp;ge;99.0%&lt;/span&gt;</td></tr></tbody></table>

synthesis of high purity nonsymmetric dialkylphosphinic acid extractants

Biz bir sentez mevcut (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) phosphinic asit yüksek saflıkta nonsymmetric dialkylphosphinic asit extractants sentezi için bir yöntem göstermek için bir örnek olarak. Düşük toksik sodyum hipofosfit bir (2,3-Dimetil-1-monoalkylphosphinic asit ara oluşturmak için butene) organik ile tepki için fosfor kaynağı olarak seçilmiştir. Sadece monoalkylphosphinic asit dialkylphosphinic asit ile Amantadin nedeniyle tepki değil iken bir amantadine∙mono-alkylphosphinic asit tuz formu Amantadin ile tepki olarak Amantadin dialkylphosphinic asit yan ürünü kaldırmak için kabul edildi onun büyük steric engel. Saf monoalkylphosphinic asit sonra organik nonsymmetric dialkylphosphinic asit (NSDAPA) vermeye B (diisobutylene) ile tepki. Unreacted monoalkylphosphinic asit-ebilmek var olmak kolayca çıkarmak bir basit Bankası-asit tarafından tedavi sonrası ve diğer organik kirleri kobalt tuzu yağış ayrılabilir. Yapısı (2, 3-dimethylbutyl) (2,4, 4'-trimethylpentyl) phosphinic asit olduğunu doğruladı 31P NMR, 1H NMR, ESI-MS ve FT-IR. tarafından Saflık potentiometric titrasyon yöntemi tarafından tespit edildi ve saflığı % 96 aşabilir sonuçlar gösterir.

31 P NMR spektrumları için mono-(2,3-dimethylbutyl) phosphinic asit önce ve sonra arıtma Amantadin yöntemi (Resim 1a-b) tarafından toplanmıştır. 31 P NMR spectra, 1H NMR spectra, MS spectra ve FT-IR spektrumları için toplanan (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) phosphinic asit (bkz şekil 3, şekil 4, şekil 5...

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

Yüksek saflıkta Nonsymmetric Dialkylphosphinic asit Extractants sentezi

Alarak yüksek saflıkta nonsymmetric dialkylphosphinic asit extractants sentezi için bir protokol sunulmuştur (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) bir örnek olarak phosphinic asit.

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 Görüntüleme.  University of Science and Technology Beijing. Alarak yüksek saflıkta nonsymmetric dialkylphosphinic asit extractants sentezi için bir protokol sunulmuştur (2,3-dimethylbutyl) (2,4, 4'-trimethylpentyl) bir örnek olarak phosphinic asit.

Video: Synthesis of High Purity Nonsymmetric Dialkylphosphinic Acid Extractants

Compact Quantum Dots for Single-molecule Imaging

Single-molecule imaging is an important tool for understanding the mechanisms of biomolecular function and for visualizing the spatial and temporal heterogeneity of molecular behaviors that underlie cellular biology 1-4. To image an individual molecule of interest, it is typically conjugated to a fluorescent tag (dye, protein, bead, or quantum dot) and observed with epifluorescence or total internal reflection fluorescence (TIRF) microscopy. While dyes and fluorescent proteins have been the mainstay of fluorescence imaging for decades, their fluorescence is unstable under high photon fluxes necessary to observe individual molecules, yielding only a few seconds of observation before complete loss of signal. Latex beads and dye-labeled beads provide improved signal stability but at the expense of drastically larger hydrodynamic size, which can deleteriously alter the diffusion and behavior of the molecule under study.
Quantum dots (QDs) offer a balance between these two problematic regimes. These nanoparticles are composed of semiconductor materials and can be engineered with a hydrodynamically compact size with exceptional resistance to photodegradation 5. Thus in recent years QDs have been instrumental in enabling long-term observation of complex macromolecular behavior on the single molecule level. However these particles have still been found to exhibit impaired diffusion in crowded molecular environments such as the cellular cytoplasm and the neuronal synaptic cleft, where their sizes are still too large 4,6,7.
Recently we have engineered the cores and surface coatings of QDs for minimized hydrodynamic size, while balancing offsets to colloidal stability, photostability, brightness, and nonspecific binding that have hindered the utility of compact QDs in the past 8,9. The goal of this article is to demonstrate the synthesis, modification, and characterization of these optimized nanocrystals, composed of an alloyed HgxCd1-xSe core coated with an insulating CdyZn1-yS shell, further coated with a multidentate polymer ligand modified with short polyethylene glycol (PEG) chains (Figure 1). Compared with conventional CdSe nanocrystals, HgxCd1-xSe alloys offer greater quantum yields of fluorescence, fluorescence at red and near-infrared wavelengths for enhanced signal-to-noise in cells, and excitation at non-cytotoxic visible wavelengths. Multidentate polymer coatings bind to the nanocrystal surface in a closed and flat conformation to minimize hydrodynamic size, and PEG neutralizes the surface charge to minimize nonspecific binding to cells and biomolecules. The end result is a brightly fluorescent nanocrystal with emission between 550-800 nm and a total hydrodynamic size near 12 nm. This is in the same size range as many soluble globular proteins in cells, and substantially smaller than conventional PEGylated QDs (25-35 nm).

We describe the preparation of colloidal quantum dots with minimized hydrodynamic size for single-molecule fluorescence imaging. Compared to conventional quantum dots, these nanoparticles are similar in size to globular proteins and are optimized for single-molecule brightness, stability against photodegradation, and resistance to nonspecific binding to proteins and cells.

Tek molekül Görüntüleme için kompakt Kuantum Noktaları

Single-molecule imaging is an important tool for  understanding the mechanisms of biomolecular function and for visualizing the  spatial and temporal ...

Mühendislik

Synthesis and Purification of Iodoaziridines Involving Quantitative Selection of the Optimal Stationary Phase for Chromatography

The highly diastereoselective preparation of cis-N-Ts-iodoaziridines through reaction of diiodomethyllithium with N-Ts aldimines is described. Diiodomethyllithium is prepared by the deprotonation of diiodomethane with LiHMDS, in a THF/diethyl ether mixture, at -78 &#176;C in the dark. These conditions are essential for the stability of the LiCHI2 reagent generated. The subsequent dropwise addition of N-Ts aldimines to the preformed diiodomethyllithium solution affords an amino-diiodide intermediate, which is not isolated. Rapid warming of the reaction mixture to 0 &#176;C promotes cyclization to afford iodoaziridines with exclusive cis-diastereoselectivity. The addition and cyclization stages of the reaction are mediated in one reaction flask by careful temperature control.
Due to the sensitivity of the iodoaziridines to purification, assessment of suitable methods of purification is required. A protocol to assess the stability of sensitive compounds to stationary phases for column chromatography is described. This method is suitable to apply to new iodoaziridines, or other potentially sensitive novel compounds. Consequently this method may find application in range of synthetic projects. The procedure involves firstly the assessment of the reaction yield, prior to purification, by 1H NMR spectroscopy with comparison to an internal standard. Portions of impure product mixture are then exposed to slurries of various stationary phases appropriate for chromatography, in a solvent system suitable as the eluent in flash chromatography. After stirring for 30 min to mimic chromatography, followed by filtering, the samples are analyzed by 1H NMR spectroscopy. Calculated yields for each stationary phase are then compared to that initially obtained from the crude reaction mixture. The results obtained provide a quantitative assessment of the stability of the compound to the different stationary phases; hence the optimal can be selected. The choice of basic alumina, modified to activity IV, as a suitable stationary phase has allowed isolation of certain iodoaziridines in excellent yield and purity.

A protocol for the diastereoselective one-pot preparation of cis-N-Ts-iodoaziridines is described. The generation of diiodomethyllithium, addition to N-Ts aldimines and cyclization of the amino gem-diiodide intermediate to iodoaziridines is demonstrated. Also included is a protocol to rapidly and quantitatively assess the most appropriate stationary phase for purification by chromatography.

Sentez ve Kromatografi için optimal sabit faz kantitatif seçimi dahil edilmesi Iodoaziridines saflaştırılması

The highly diastereoselective preparation of cis-N-Ts-iodoaziridines through reaction of diiodomethyllithium with N-Ts aldimines is described. ...

Kimya

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

Phosphopeptides Gelişmiş Zenginleştirme için Makrogözenekli Polimer Monoliths üzerinde yüksek Gözenekli Koordinasyon Polymer Coatings Hazırlanması

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

Extraction and Characterization of Surfactants from Atmospheric Aerosols

Surface-active compounds, or surfactants, present in atmospheric aerosols are expected to play important roles in the formation of liquid water clouds in the Earth&#39;s atmosphere, a central process in meteorology, hydrology, and for the climate system. But because specific extraction and characterization of these compounds have been lacking for decades, very little is known on their identity, properties, mode of action and origins, thus preventing the full understanding of cloud formation and its potential links with the Earth&#39;s ecosystems.
In this paper we present recently developed methods for 1) the targeted extraction of all the surfactants from atmospheric aerosol samples and for the determination of 2) their absolute concentrations in the aerosol phase and 3) their static surface tension curves in water, including their Critical Micelle Concentration (CMC). These methods have been validated with 9 references surfactants, including anionic, cationic and non-ionic ones. Examples of results are presented for surfactants found in fine aerosol particles (diameter &#60;1 &#956;m) collected at a coastal site in Croatia and suggestions for future improvements and other characterizations than those presented are discussed.

Methods are presented for the targeted extraction of surfactants present in atmospheric aerosols and the determination of their absolute concentrations and surface tension curves in water, including their Critical Micelle Concentration (CMC).

Atmosferik Aerosoller ekstraksiyonu ve Yüzey Aktif Karakterizasyonu

Surface-active compounds, or surfactants, present in atmospheric aerosols are expected to play important roles in the formation of liquid water clouds in ...

Çevre

Facile Protocol for the Synthesis of Self-assembling Polyamine-based Peptide Amphiphiles (PPAs) and Related Biomaterials

Polyamine-based Peptide Amphiphiles (PPAs) are a new class of self-assembling amphiphilic biomaterials-related to the peptide amphiphiles (PAs). Traditional PAs possess charged amino acids as solubilizing groups (lysine, arginine), which are directly connected to a lipid segment or can contain a linker region made of neutral amino acids. Tuning the peptide sequence of PAs can yield diverse morphologies. Similarly, PPAs possess a hydrophobic segment and neutral amino acids, but also contain polyamine molecules as water solubilizing (hydrophilic) groups. As is the case with PAs, PPAs can also self-assemble into diverse morphologies, including small rods, twisted nano-ribbons, and fused nano-sheets, when dissolved in water. However, the presence of both primary and secondary amines on a single polyamine molecule poses a significant challenge when synthesizing PPAs. In this paper, we show a simple protocol, based on literature precedents, to achieve a facile synthesis of PPAs using solid phase peptide synthesis (SPPS). This protocol can be extended to the synthesis of PAs and other similar systems. We also illustrate the steps that are needed for cleavage from the resin, identification, and purification.

Facile Protocol for the Synthesis of Self-assembling Polyamine-based Peptide Amphiphiles PPAs and Related Biomaterials

The synthesis of polyamine-based peptide amphiphiles (PPAs) is a significant challenge due to the presence of multiple amine nitrogens, which requires judicious use of protecting groups to mask these reactive functionalities. In this paper, we describe a facile method for the preparation of these new class of self-assembling molecules.

Polyamine tabanlı peptid Amphiphiles (PPAs) ve ilgili Biyomalzeme kendi kendine montaj sentezi için facile iletişim kuralı

Polyamine-based Peptide Amphiphiles (PPAs) are a new class of self-assembling amphiphilic biomaterials-related to the peptide amphiphiles (PAs). ...

Synthesis of Esters Via a Greener Steglich Esterification in Acetonitrile

The Steglich esterification is a widely-used reaction for the synthesis of esters from carboxylic acids and alcohols. While efficient and mild, the reaction is commonly performed using chlorinated or amide solvent systems, which are hazardous to human health and the environment. Our methodology utilizes acetonitrile as a greener and less hazardous solvent system. This protocol exhibits rates and yields that are comparable to traditional solvent systems and employs an extraction and wash sequence that eliminates the need for the purification of the ester product via column chromatography. This general method can be used to couple a variety of carboxylic acids with 1&#176; and 2&#176; aliphatic alcohols, benzylic and allylic alcohols, and phenols to obtain pure esters in high yields. The goal of the protocol detailed here is to provide a greener alternative to a common esterification reaction, which could serve useful for ester synthesis in both academic and industrial applications.

A modified Steglich esterification reaction was used to synthesize a small library of ester derivatives with primary and secondary alcohols. The methodology uses a non-halogenated and greener solvent, acetonitrile, and enables product isolation in high yields without the need for chromatographic purification.

Esterleri bir yeşil Steglich esterleşme Asetonitril içinde yolu ile sentezi

The Steglich esterification is a widely-used reaction for the synthesis of esters from carboxylic acids and alcohols. While efficient and mild, the ...

Preparation of Poly(pentafluorophenyl acrylate) Functionalized SiO2 Beads for Protein Purification

We demonstrate a simple method to prepare poly(pentafluorophenyl acrylate) (poly(PFPA)) grafted silica beads for antibody immobilization and subsequent immunoprecipitation (IP) application. The poly(PFPA) grafted surface is prepared via a simple two-step process. In the first step, 3-aminopropyltrimethoxysilane (APTMS) is deposited as a linker molecule onto the silica surface. In the second step, poly(PFPA) homopolymer, synthesized via the reversible addition and fragmentation chain transfer (RAFT) polymerization, is grafted to the linker molecule through the exchange reaction between the pentafluorophenyl (PFP) units on the polymer and the amine groups on APTMS. The deposition of APTMS and poly(PFPA) on the silica particles are confirmed by X-ray photoelectron spectroscopy (XPS), as well as monitored by the particle size change measured via dynamic light scattering (DLS). To improve the surface hydrophilicity of the beads, partial substitution of poly(PFPA) with amine-functionalized poly(ethylene glycol) (amino-PEG) is also performed. The PEG-substituted poly(PFPA) grafted silica beads are then immobilized with antibodies for IP application. For demonstration, an antibody against protein kinase RNA-activated (PKR) is employed, and IP efficiency is determined by Western blotting. The analysis results show that the antibody immobilized beads can indeed be used to enrich PKR while non-specific protein interactions are minimal.

Preparation of Polypentafluorophenyl acrylate Functionalized SiO2 Beads for Protein Purification

A protocol for the preparation of poly(pentafluorophenyl acrylate) (poly(PFPA)) grafted silica beads is presented. The poly(PFPA) functionalized surface is then immobilized with antibodies and used successfully for the protein separation through immunoprecipitation.

Poly(pentafluorophenyl acrylate) Functionalized SiO2 boncuk hazırlanması için Protein Saflaştırma

We demonstrate a simple method to prepare poly(pentafluorophenyl acrylate) (poly(PFPA)) grafted silica beads for antibody immobilization and subsequent ...

Enzymatic Synthesis of Epoxidized Metabolites of Docosahexaenoic, Eicosapentaenoic, and Arachidonic Acids

The epoxidized metabolites of various polyunsaturated fatty acids (PUFAs), termed epoxy fatty acids, have a wide range of roles in human physiology. These metabolites are produced endogenously by the cytochrome P450 class of enzymes. Because of their diverse and potent biological effects, there is considerable interest in studying these metabolites. Determining the unique roles of these metabolites in the body is a difficult task, as the epoxy fatty acids must first be obtained in significant amounts and with high purity. Obtaining compounds from natural sources is often labor intensive, and soluble epoxide hydrolases (sEH) rapidly hydrolyze the metabolites. On the other hand, obtaining these metabolites via chemical reactions is very inefficient, due to the difficulty of obtaining pure regioisomers and enantiomers, low yields, and extensive (and expensive) purification. Here, we present an efficient enzymatic synthesis of 19(S),20(R)- and 16(S),17(R)-epoxydocosapentaenoic acids (EDPs) from DHA via epoxidation with BM3, a bacterial CYP450 enzyme isolated originally from Bacillus megaterium (that is readily expressed in Escherichia coli). Characterization and determination of purity is performed with nuclear magnetic resonance spectroscopy (NMR), high-performance liquid chromatography (HPLC), and mass spectrometry (MS). This procedure illustrates the benefits of enzymatic synthesis of PUFA epoxy metabolites, and is applicable to the epoxidation of other fatty acids, including arachidonic acid (AA) and eicosapentaenoic acid (EPA) to produce the analogous epoxyeicosatrienoic acids (EETs) and epoxyeicosatetraenoic acids (EEQs), respectively.

We present a method useful for large-scale enzymatic synthesis and purification of specific enantiomers and regioisomers of epoxides of arachidonic acid (AA), docosahexaenoic acid (DHA), and eicosapentaenoic acid (EPA) with the use of a bacterial cytochrome P450 enzyme (BM3).

Dokosahexaenoic, eicosapentaenoic ve Arachidonik asitlerin Epoxilenmiş metabolitlerinin enzimatik sentezini

The epoxidized metabolites of various polyunsaturated fatty acids (PUFAs), termed epoxy fatty acids, have a wide range of roles in human physiology. These ...

Preparation of Contiguous Bisaziridines for Regioselective Ring-Opening Reactions

Aziridines, a class of reactive organic molecules containing a three-membered ring, are important synthons for the synthesis of a large variety of functionalized nitrogen-containing target compounds through the regiocontrolled ring-opening of C-substituted aziridines. Despite the tremendous progress in aziridine synthesis over the past decade, accessing contiguous bisaziridines efficiently remains difficult. Therefore, we were interested in synthesizing contiguous bisaziridines bearing an electronically diverse set of N-substituents beyond the single aziridine backbone for regioselective ring-opening reactions with diverse nucleophiles. In this study, chiral contiguous bisaziridines were prepared by organocatalytic asymmetric aziridination of chiral (E)-3-((S)-1-((R)-1-phenylethyl)aziridin-2-yl)acrylaldehyde with N-Ts-O-tosyl or N-Boc-O-tosyl hydroxylamine as the nitrogen source in the presence of (2S)-[diphenyl(trimethylsilyloxy)methyl]pyrrolidine as a chiral organocatalyst. Also demonstrated here are representative examples of regioselective ring-opening reactions of contiguous bisaziridines with a variety of nucleophiles such as sulfur, nitrogen, carbon, and oxygen, and the application of contiguous bisaziridines to the synthesis of multi-substituted chiral pyrrolidines by Pd-catalyzed hydrogenation.

Contiguous bisaziridines containing non-activated and activated aziridines were synthesized by asymmetric organocatalytic aziridinations and then subjected to chemoselective ring-opening reactions under acidic or basic conditions. The non-activated aziridine ring opens with less reactive nucleophiles under acidic conditions, whereas the activated aziridine ring opens with more reactive nucleophiles under basic conditions.

Regioselektif halka açma reaksiyonları için bitişik bisaziridinlerin hazırlanması

Aziridines, a class of reactive organic molecules containing a three-membered ring, are important synthons for the synthesis of a large variety of ...

Depolymerizable Olefinic Polymers Based on Fused-Ring Cyclooctene Monomers

The growing consumption of synthetic polymers and the accumulation of polymer waste have led to a pressing need for new routes to sustainable materials. Achieving a closed-loop polymer economy via chemical recycling to monomer (CRM) is one such promising route. Our group recently reported a new CRM system based on polymers prepared by ring-opening metathesis polymerization (ROMP) of trans-cyclobutane fused cyclooctene (tCBCO) monomers. This system offers several key advantages, including the ease of polymerization at ambient temperatures, quantitative depolymerization to monomers under mild conditions, and a broad range of functionalities and thermomechanical properties. Here, we outline detailed protocols for the preparation of tCBCO-based monomers and their corresponding polymers, including the preparation of elastic polymer networks and compression molding of linear thermoplastic polymers. We also outline the preparation of high ring strain E-alkene tCBCO monomers and their living polymerization. Finally, the procedures for the depolymerization of linear polymers and polymer networks are also demonstrated.

Here, we describe protocols for the preparation of trans-cyclobutane fused cyclooctenes (tCBCO),&#160;their polymerization to prepare depolymerizable olefinic polymers, and the depolymerization of these polymers under mild conditions. Additionally, protocols for the preparation of depolymerizable networks and compression molding of rigid linear plastics based on this system are described.

Kaynaşmış Halka Siklookten Monomerlerine Dayanan Depolimerize Edilebilir Olefinik Polimerler

The growing consumption of synthetic polymers and the accumulation of polymer waste have led to a pressing need for new routes to sustainable materials. ...