Este trabalho foi apoiado pela nacional natureza Science Foundation da China (21301104), os fundos de pesquisa Fundamental para as universidades Central (FRF-TP-16-019A3) e o estado chave laboratório de engenharia química (SKL--14A04).

1. síntese de Mono-(2,3-dimethylbutyl) ácido fosfínico 18 , 19 <ol><li>reação <ol><li>pesar 31,80 g hidrato de hipofosfito de sódio, 16,00 g de ácido acético, 8,42 g 2,3-dimetil-1-buteno, 0,73 g di - terc-butylnperoxide (DTBP) e g 25,00 tetrahidrofurano (THF) em um autoclave inox Teflon revestido de 100 mL, colocar um agitador magnético em autoclave e selá-lo</li>
		<li>Colocar o autoclave em uma fornalha de tubo vertical, que sob a qual é uma stirringapparatus magnética. Iniciar o aparelho de agitação magnético e definir a velocidade em rpm 800.</li>
		<li>Definir o programa de aquecimento do controlador de temperatura ligado a autoclave: calor da temperatura de 120 ° C durante 90 min, manter a 120 ° C para 8 h e, em seguida, esfriar a temperatura ambiente, naturalmente. Iniciar o programa de aquecimento.</li>
	</ol></li> <li>Pós-tratamento <ol><li>transferir os produtos para um balão de fundo redondo de um pescoço de 250 mL, lavar o forro de Teflon com 50 mL THF e adicioná-lo para o mesmo balão para garantir que todos os produtos são transferidos.</li>
		<li>Remover o THF e olefinas não tenha reagidas usando um evaporador rotativo.</li>
		<li>Transferir os resíduos em uma ampola de decantação de 250 mL, lavar o balão com éter etílico de 80 mL e 30 mL de água desionizada, respectivamente e adicioná-los para a mesma ampola de decantação para garantir que todos os produtos são transferidos.</li>
		<li>Adicionar 50 mL de solução de NaOH 4% dentro do funil de separação acima, agitá-lo vigorosamente e separar a fase aquosa. Extrair a fase orgânica com soluções de NaOH 4% 20 mL por três vezes (20 mL × 3) para garantir que a fase aquosa superior pH 10.</li>
		<li>Combinar as soluções aquosas na etapa acima e transferi-los para uma ampola de decantação de 500 mL.</li>
		<li>Adicionar 90 mL de 10% H 2 para 4 solução 50 mL de éter etílico, agitar vigorosamente e separar a fase orgânica; em seguida, extrair a fase aquosa com 30 mL de éter etílico, por três vezes (30 mL × 3).</li>
		<li>Combinar as soluções de éter etílico na etapa 1.2.6 e transferi-los para outra ampola de decantação de 500 mL.</li>
		<li>Lavá-lo com 100 mL de soluções saturadas de NaCl quatro vezes (100 mL × 4).</li>
		<li>Adicionar 4G de anidro MgSO 4 para remover qualquer solúvel em água. Filtro para remover o sólido e recolher o líquido em um balão de fundo redondo de um pescoço limpo de 250 mL.</li>
		<li>Remover o éter etílico usando o evaporador rotativo para obter 17,92 g do produto bruto.</li>
	</ol></li></ol> 2. Purificação de Mono-(2,3-dimethylbutyl) ácido fosfínico <ol><li>preparação da solução de Amantadina <ol><li>dissolver 22,28 g de cloridrato de Amantadina em 100 mL de água desionizada num copo de 500 mL.</li>
		<li>Adicionar 100 mL de saturado de solução de NaOH e mexa por 5 min.</li>
		<li>Adicionar 150 mL de éter etílico e mexa até que o precipitado branco gerado na etapa 2.1.2 desaparece.</li>
		<li>Transferir as soluções para uma ampola de decantação de 500 mL, lavar o copo com éter etílico por três vezes (50 mL × 3) e combiná-los para a mesma ampola de decantação.</li>
		<li>Separar a fase aquosa e lave a fase orgânica com soluções saturadas de NaCl cinco vezes (100 mL × 5).</li>
		<li>Adicionar 4G de anidro MgSO 4 para remover qualquer solúvel em água. Filtro para obter a solução de éter etílico Amantadina.</li>
	</ol></li> <li>Preparação de Amantadina &#8729; mono-(2,3-dimethylbutyl) sal ácido fosfínico <ol><li>drop-wise adicionar o produto fosfínico ácido mono bruto-(2,3-dimethylbutyl) a solução de Amantadina. Durante a queda adicionar 150 mL de éter etílico para garantir que ele pode mexer corretamente.</li>
		<li>Lavar o pescoço um balão contendo o mono-(2,3-dimethylbutyl) fosfínico produto ácido com 50 mL de éter etílico para garantir que todo o produto é transferido para a solução de Amantadina. Mexa por 30 min e deixe descansar durante a noite.</li>
		<li>Filtro abaixo dos reduziu a pressão e lavar a torta de filtro com éter etílico de 200 mL.</li>
	</ol></li> <li>Liberar o ácido fosfínico mono-(2,3-dimethylbutyl) <ol><li>transferir o bolo filtrado em um béquer de 500 mL, adicione 80 mL de 1 HCl, M e mexa por 5 min.</li>
		<li>Adicionar 70 mL de acetato de etilo e mexa mais 5 min.</li>
		<li>Transferir as soluções para uma ampola de decantação de 250 mL e separar a fase aquosa.</li>
		<li>Extrair a fase aquosa com 40 mL de acetato de etilo novamente e combinar as soluções de acetato de etila.</li>
		<li>Lavar a solução de acetato de etila com 30 mL de 1 HCl, M duas vezes (30 mL × 2) e saturada de NaCl três vezes (80 mL × 3), sequencialmente.</li>
		<li>Adicionar 4G anidro MgSO 4 para remover qualquer solúvel em água. Filtrar e recolher o líquido em um balão de fundo redondo de um pescoço de 250 mL.</li>
		<li>Remover o acetato de etilo usando o evaporador rotativo e obter 12,45 g do ácido fosfínico pura mono-(2,3-dimethylbutyl) (rendimento: 82,9%).</li>
	</ol></li></ol> 3. Síntese de (2,3-dimethylbutyl) (2, 4,4 &#39;-trimetilpentil) ácido fosfínico <ol><li>reação <ol><li>transferência todas do puro mono-(2,3-dimethylbutyl) fosfínico ácido produto em 100 mL, um Teflon revestido aço inoxidável autoclave, adicionar 4,95 g de ácido acético, 25,39 g de diisobutylene, 0,30 g de DTBP, colocar um agitador magnético em autoclave e selá-lo</li>
		<li>Colocar o autoclave em uma fornalha de tubo vertical, sob o qual é um instrumento de agitação magnético, e iniciar o aparelho agitação magnético.</li>
		<li>Definir o programa de aquecimento do controlador de temperatura: calor da temperatura de 135 ° C durante 90 min, manter a 135 ° C, durante 8 h e, em seguida, esfriar a temperatura ambiente, naturalmente. Iniciar o programa de aquecimento.</li>
		<li>Quando o sistema de reação arrefece à temperatura ambiente, adicione outra 0,30 g de DTBP e reinicie o programa de aquecimento.</li>
		<li>Repita uma vez o passo 3.1.4.</li>
	</ol></li> <li>Pós-tratamento <ol><li>diluir o produto com 100 mL de éter de etilo e depois transferir para uma ampola de decantação de 250 mL.</li>
		<li>Lavá-lo com 30 mL de 4% NaOH três vezes (30 mL × 3) para garantir que a fase aquosa excede pH 10.</li>
		<li>Adicionar 70 mL de 10% H 2 então 4 solução para acidificar o produto.</li>
		<li>Lavá-lo com solução saturada de NaCl várias vezes (80 mL cada uma) até que o pH da fase aquosa é igual a pH 6-7.</li>
		<li>Adicionar 4G de anidro MgSO 4 para remover qualquer solúvel em água. Filtro para remover o sólido e recolher o líquido em um balão de fundo redondo de um pescoço limpo de 250 mL.</li>
		<li>Remover o éter etílico e olefinas não tenha reagidas usando o evaporador rotativo para obter 15,10 g de produto bruto.</li>
	</ol></li></ol> 4. Purificação de (2,3-dimethylbutyl) (2, 4,4 &#39;-trimetilpentil) ácido fosfínico <ol><li>obter co-(2,3-dimethylbutyl) puro (2, 4,4 &#39;-trimetilpentil) ácido fosfínico complexo <ol><li>dissolver 2,30 g de NaOH em 40 mL água desionizada. Adicionar a solução de NaOH no balão contendo o petróleo bruto (2,3-dimethylbutyl) (2, 4,4 &#39;-trimetilpentil) produto ácido fosfínico e agitar vigorosamente durante 5 min.</li>
		<li>Adicionar 0,5 M CoCl 2 solução gota a gota agitando até que não mais precipitado azul é gerado e a solução no frasco rosa. < / li> <li>Filtro e lave o precipitado azul com água desionizada até a torta de filtro é incolor.</li>
		<li>Transferir a torta de filtro para um copo de 250 mL, adicionar 100 mL de acetona, selá-lo com película conservante e então ele refrigerar a 4 ° C por uma noite.</li>
		<li>Pulverize o precipitado azul para liberar as impurezas presas a granel.</li>
		<li>Filtro e lave-o com 100 mL de acetona fresca. Secar a torta de filtro à temperatura ambiente e em seguida, transferi-lo para uma ampola de decantação de 250 mL.</li>
	</ol></li> <li>Regenerar o (2,3-dimethylbutyl) (2, 4,4 &#39;-trimetilpentil) ácido fosfínico <ol><li>Adicionar 120 mL éter etílico e 80 mL 10% H 2 para 4 e agitar vigorosamente até o precipitado azul desaparece....</li>
		<li>Separar a fase aquosa, lavar o orgânico fase sequencialmente com 30 mL de 10% H 2 SO 4 uma vez e saturada soluções de NaCl (80 mL cada) de várias vezes até que o pH da fase aquosa é igual a pH 6-7.</li>
		<li>Adicionar 4G de anidro MgSO 4 para remover qualquer solúvel em água. Filtro para remover o sólido e recolher o líquido em um balão de fundo redondo de um pescoço limpo de 250 mL.</li>
		<li>Remover o éter etílico usando o evaporador rotativo e obter 11,46 g do produto puro (rendimento: 52,8%).</li>
	</ol>
	</li>
</ol>

<ol>
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Os autores não têm nada para divulgar.

O passo mais crítico no âmbito do protocolo é o ácido mono-alkylphosphinic síntese (Figura 1um). Nesta reação, um maior rendimento e menos subproduto de ácido dialkylphosphinic é melhor. Aumentando a proporção molar do NaH2PO2/olefin A melhorar o rendimento e inibir a geração de um subproduto de ácido dialkylphosphinic. No entanto, uma grande NaH2PO2 dosagem também vai aumentar o custo e causar um problema de agitaç...

Ácido extractants organofosforados são amplamente utilizados no campo tradicional hidrometalurgia para extração e separação de íons de terras raras1,2, metais não-ferrosos (como Co/Ni3,4), metais raros ( como Hf/Zr5, V.6,7), actinídeos8, etc. Nos últimos anos, eles também têm atraído mais atenção nas áreas de recursos secundários reciclagem e eliminação de resíduos líquidos de alto nível9. Di-(2-etil-hexil) fosfórico (D2EHPA ou P204), 2-ethylhexylphosphoric ácido mono-2-etilhexil éster (EHEHPA, PC 88A ou P507) e Di-(2,4, 4'-trimetilpentil)-ácido fosfínico (Cyanex272), que são representantes de ácidos dialkylphosphoric, alkylphosphoric ácido mono-alquil ésteres e os ácidos dialkylphosphinic respectivamente, são os mais comumente usados extratores. Sua acidez diminui na seguinte sequência: P204 &#62; P507 &#62; Cyanex 272. A correspondente capacidade de extração, a capacidade de extração e acidez descascamento são tudo na ordem P204 &#62; P507 &#62; Cyanex 272 e o desempenho de separação é na ordem oposta. Estes três extratores são eficazes na maioria dos casos. No entanto, ainda existem algumas condições onde eles não são tão eficientes: na separação pesado terras raras, das quais os principais problemas existentes são a seletividade pobre e alta acidez descascamento para P204 e P507, baixa capacidade de extração e tendência de emulsão durante a extração para Cyanex 272. Assim, o desenvolvimento de extratores novela tem chamado a atenção maior nos últimos anos.
A classe de dialkylphosphinic ácido extractants é considerada ser um dos aspectos mais importantes pesquisas para desenvolver novos extratores. Pesquisas recentes mostraram que a capacidade de extração de ácidos dialkylphosphinic depende em grande parte da estrutura do alquilo substituintes10,11. Pode ser uma grande variedade de significativamente maior que a de P507 para abaixar do que o de Cyanex 27212. No entanto, a exploração do romance dialkylphosphinic ácido extractants é restrito para o comercial do olefin estrutura10,12,13,14,15, 16. Embora dialkylphosphinic ácido extractants também podem ser sintetizados pelo método da reação de Grignard, as condições da reação são rigorosos12,17.
NSDAPA, dos quais os dois alquilos são diferentes, abre uma porta para a exploração de novos extratores. Isso faz com que as estruturas de ácido dialkylphosphinic mais diversificada, e seu desempenho de extração e separação pode aperfeiçoá-lo, modificando tanto das suas estruturas de alquila. O tradicional método sintético de NSDAPA usado PH3 como uma fonte de fósforo, que tem muitas desvantagens como alta toxicidade, condições da reação rigorosa e difícil purificação. Recentemente, informou um novo método para sintetizar NSDAPA usando hipofosfito de sódio como um fósforo de origem (ver Figura 1) e sintetizados com sucesso três NSDAPAs18. Este protocolo detalhado pode ajudar novos praticantes repetir as experiências e dominar o método sintético de extratores NSDAPA. Tomamos (2,3-dimethylbutyl) (2,4, 4'-trimetilpentil) ácido fosfínico como exemplo. Os nomes e estruturas do olefin A, o ácido mono-alkylphosphinic intermediário, olefin B e o correspondente NSDAPA são mostradas na tabela 1.

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		<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

Apresentamos a síntese de (2,3-dimethylbutyl) (2,4, 4'-trimetilpentil) ácido fosfínico como exemplo para demonstrar um método para a síntese de alta pureza da gravitação assimétrica dialkylphosphinic ácido extractants. Hipofosfito de sódio baixo tóxico foi escolhido como a fonte de fósforo para reagir com olefinas um (2,3-dimetil-1-buteno) para gerar um ácido monoalkylphosphinic intermediário. Amantadina foi adotada para remover o subproduto de ácido dialkylphosphinic, pois apenas o ácido monoalkylphosphinic pode reagir com amantadina para formar um sal de ácido amantadine∙mono-alkylphosphinic, enquanto o ácido dialkylphosphinic não pode reagir com amantadina devido a sua grande estérico. O ácido monoalkylphosphinic purificado foi então reagiu com olefinas B (diisobutylene) para produzir ácido dialkylphosphinic da gravitação assimétrica (NSDAPA). O ácido monoalkylphosphinic não tenha reagido pode ser facilmente removido por um simples pós-tratamento base-ácido e outras impurezas orgânicas podem ser separadas para fora através da precipitação do sal de cobalto. A estrutura da (2,3-dimethylbutyl) (2,4, 4'-trimetilpentil) ácido fosfínico foi confirmado por NMR 31P, 1H NMR, ESI-MS e FT-ir A pureza foi determinada por um método de titulação potenciométrica, e os resultados indicam que a pureza pode exceder 96%.

31 Espectros de RMN de P foram coletados para o mono-(2,3-dimethylbutyl) ácido fosfínico antes e após a purificação pelo método de amantadina (Figura 1a-b). 31 Espectros de RMN de P, espectro de RMN de H 1, espectros de MS e espectros de FT-IR foram coletados para (2,3-dimethylbutyl) (2,4, 4'-trimetilpentil) ácido fosfínico (ver Figura 3, Figura 4</str...

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

Síntese de alta pureza da gravitação assimétrica Dialkylphosphinic ácido Extractants

É apresentado um protocolo para a síntese de alta pureza da gravitação assimétrica dialkylphosphinic ácido extractants, tomando (2,3-dimethylbutyl) (2,4, 4'-trimetilpentil) ácido fosfínico como exemplo.

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 visualizações.  University of Science and Technology Beijing. É apresentado um protocolo para a síntese de alta pureza da gravitação assimétrica dialkylphosphinic ácido extractants, tomando (2,3-dimethylbutyl) (2,4, 4'-trimetilpentil) ácido fosfínico como exemplo.

Vídeo: 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.

Síntese de Antiviral tetrahidrocarbazole Derivativos por fotoquímica e catalisada por ácido CH funcionalização via Peróxidos intermediários (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 ...

Química

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.

Síntese de Immunotargeted magneto-plasmónico Nanoclusters

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.

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.

Síntese e Caracterização de Supramoleculares Colloids

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.

Hidroquinona baseada Síntese de ouro 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.

Síntese de hierárquicos 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.

Método de precipitação química para a síntese do Nb2O5 modificado catalisadores de níquel em massa com alta área de superfície específica

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.

Síntese de nanofios de Au substrato ligados através de um mecanismo de crescimento ativo de superfície

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.

Fase sólida síntese de [4,4] Spirocyclic oximas

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.

Síntese e caracterização de nanopartículas de ouro Anfífilos

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