这项工作得到了中国国家自然科学基金 (21301104)、中央大学基础研究基金 (FRF-TP-16-019A3) 和国家重点化学工程实验室 (SKL-ChE-14A04) 的支持。

1. 单 (23-dimethylbutyl) 膦酸的合成 18 , 19 <ol> <li> 反应 <ol> <li> 重 31.80 g 磷酸钠次水合物, 16.00g 乙酸, 8.42 克 23-二甲基-1-丁烯, 0.73 g di- 叔 butylnperoxide (DTBP), 和25.00 克四氢呋喃 (呋喃) 成100毫升聚四氟乙烯内衬不锈钢高压釜, 把一个磁力搅拌器放入高压釜, 并密封它. </li>
		<li> 将高压釜置于垂直管式炉中, 其下是磁性 stirringapparatus。启动磁搅拌装置, 设置速度在 800 rpm. </li>
		<li> 设置连接到高压釜的温度控制器的加热程序: 室温到120和 #176; c 在90分钟内, 保持120和 #176; c 为8小时, 然后自然地冷却到室温。启动加热程序. </li>
	</ol> </li> <li> 后处理 <ol> <li> 将产品转换为250毫升的单颈圆底烧瓶, 用50毫升呋喃清洗聚四氟乙烯衬里, 并将其添加到同一烧瓶中, 以确保所有产品均已转移. </li>
		<li> 使用旋转式蒸发器去除呋喃和未烯烃. </li>
		<li> 将残渣转化为250毫升分离漏斗, 分别用80毫升乙醚和30毫升去离子水冲洗烧瓶, 并将其放入相同的分离漏斗中, 以确保所有产品都被转移. </li>
		<li> 在上述分离漏斗中加入50毫升4% 氢氧化钠溶液, 用力摇动, 并分离水相。用20毫升4% 氢氧化钠溶液萃取三次 (20 毫升和 #215 3) 的有机相, 以确保水相超过 pH 值 10. </li>
		<li> 在上述步骤中结合水溶液, 并将其转化为500毫升分离漏斗. </li>
		<li> 添加 90 ml 10% H 2 所以 4 溶液和50毫升乙醚, 用力摇动, 并分离有机相; 然后用30毫升乙醚提取水相三次 (30 毫升和 #215; 3)。
		<li> 将乙醚溶液在阶梯1.2.6 中结合, 并将其转移到另外500毫升分离漏斗中. </li>
		<li> 用100毫升饱和 NaCl 溶液洗涤四次 (100 毫升和 #215; 4). </li>
		<li> 添加4克无水 MgSO 4 去除任何水溶性水。过滤器, 以消除固体, 并收集液体在一个干净的250毫升单颈部圆底烧瓶. </li>
		<li> 用旋转蒸发器将乙醚取出以获得17.92 克的原油产品. </li>
	</ol> </li> </ol> 2。纯化单 (23-dimethylbutyl) 膦酸 <ol> <li> 制备金刚烷胺溶液 <ol> <li> 在 500 ml 烧杯中的100毫升去离子水中溶解22.28 克胺烷胺胺. </li>
		<li> 加入100毫升饱和氢氧化钠溶液, 搅拌5分钟. </li>
		<li> 加入150毫升乙醚, 并搅拌, 直到白色沉淀产生的步骤2.1.2 消失. </li>
		<li> 将解决方案转换为500毫升分离漏斗, 用乙醚洗涤烧杯三次 (50 毫升和 #215; 3), 并将它们组合成相同的分离漏斗. </li>
		<li> 分离水相, 用饱和 NaCl 溶液洗涤有机相中五次 (100 毫升和 #215; 5). </li>
		<li> 添加4克无水 MgSO 4 去除任何水溶性水。过滤器获得金刚烷胺乙醚溶液. </li>
	</ol> </li> <li> 制备金刚烷胺和 #8729; 单 (23-dimethylbutyl) 膦酸盐 <ol> <li> 将 drop-wise 的粗单 (23-dimethylbutyl) 膦酸产品添加到金刚烷胺溶液中。在滴加150毫升乙醚, 以确保它可以正常搅拌. </li>
		<li> 用50毫升乙醚清洗单颈圆底烧瓶, 其中含有 23-dimethylbutyl) 膦酸产品, 确保将所有产品转移到金刚烷胺溶液中。搅拌30分钟, 让它坐一夜. </li>
		<li> 在减压下过滤, 用200毫升乙醚清洗滤饼. </li>
	</ol> </li> <li> 释放单声道 (23-dimethylbutyl) 膦酸 <ol> <li> 将过滤后的蛋糕转换为500毫升的烧杯, 添加80毫升的 1 M HCl, 并搅拌5分钟. </li>
		<li> 添加70毫升乙酸乙酯, 然后再搅拌5分钟. </li>
		<li> 将解决方案转换为250毫升分离漏斗并分离水相. </li>
		<li> 再次提取40毫升乙酸乙酯的水相, 并结合乙酸乙酯溶液. </li>
		<li> 以30毫升1米 HCl (30 毫升和 #215; 2) 和饱和 NaCl 三次 (80 毫升和 #215; 3) 依次冲洗乙酸乙酯溶液. </li>
		<li> 添加4克无水 MgSO 4 去除任何水溶性水。在一个250毫升的单颈圆底烧瓶中过滤和收集液体. </li>
		<li> 使用旋转式蒸发器取出乙酸乙酯, 并获得12.45 克纯单 (23-dimethylbutyl) 膦酸 (产量: 82.9%). </li>
	</ol> </li> </ol> 3。合成 (23-dimethylbutyl) (24, 4 和 #39;-2,4,4-) 膦酸 <ol> <li> 反应 <ol> <li> 将所有纯单 (23-dimethylbutyl) 膦酸产品转换为100毫升聚四氟乙烯内衬不锈钢高压釜, 加入4.95 克乙酸, 25.39 克丁烯, 0.30 克 DTBP, 将磁力搅拌器放入高压釜, 密封. </li>
		<li> 将高压釜放在垂直管式炉中, 其中有磁性搅拌装置, 启动磁力搅拌装置. </li>
		<li> 设置温度控制器的加热程序: 室温到135和 #176; c 在90分钟内, 保持在135° c, 在8小时内, 然后自然冷却到室温。启动加热程序. </li>
		<li> 当反应系统冷却到室温时, 再加0.30 克 DTBP, 重新启动加热程序. </li>
		<li> 重复步骤3.1.4 一次. </li>
	</ol> </li> <li> 后处理 <ol> <li> 将产品与100毫升乙醚稀释, 然后转到250毫升分离漏斗。
		<li> 冲洗30毫升4% 氢氧化钠三次 (30 毫升和 #215; 3), 以确保水相超过 pH 10. </li>
		<li> 添加 70 mL 10% H 2 所以 4 解决方案以酸化该产品. </li>
		<li> 用饱和 NaCl 溶液冲洗几次 (每次80毫升), 直到水相 ph 值等于 ph 值 6-7. </li>
		<li> 添加4克无水 MgSO 4 去除任何水溶性水。过滤器, 以消除固体, 并收集液体在一个干净的250毫升单颈部圆底烧瓶. </li>
		<li> 使用旋转蒸发器将乙醚和未烯烃除去, 以获得15.10 克的原油产品. </li>
	</ol> </li> </ol> 4。纯化 (23-dimethylbutyl) (24、4和 #39;-2,4,4-) 膦酸 <ol> <li> 获得纯 co (23-dimethylbutyl) (24、4和 #39;-2,4,4-) 膦酸络合物 <ol> <li> 2.30 毫升中溶解40克氢氧化钠去离子水。在含有粗 (23-dimethylbutyl) (24、4和 #39;-2,4,4-) 膦酸产品的烧瓶中加入氢氧化钠溶液, 用力摇动5分钟. </li>
		<li> 添加 0.5 M CoCl 2 解决方案滴, 而在摇晃直到没有更多的蓝色沉淀产生, 并在瓶子里的解决方案是粉红色。>> <li> 过滤和洗涤蓝色沉淀与去离子水, 直到滤饼是无色的. </li>
		<li> 将滤饼放入一个250毫升的烧杯中, 加入100毫升丙酮, 用保鲜膜封住, 然后在4和 #176 冷藏; 一晚. </li>
		<li> 粉碎蓝色沉淀物以释放在散装中捕获的任何杂质. </li>
		<li> 过滤和清洗100毫升新鲜丙酮。在室温下烘干滤饼, 然后将其转化为250毫升分离漏斗. </li>
	</ol> </li> <li> 可再生 (23-dimethylbutyl) (24、4和 #39;-2,4,4-) 膦酸 <ol> <li> 添加120毫升乙醚和 80 ml 10% H 2 所以 4 , 然后用力摇动直到蓝色沉淀消失. </li>
		<li> 分离水相, 连续洗涤有机阶段以30毫升 10% H 2 所以 4 一次和饱和 NaCl 溶液多次 (80 毫升) 直到水相 ph 等于 ph 6-7. </li>
		<li> 添加4克无水 MgSO 4 去除任何水溶性水。过滤器, 以清除固体和收集液体在一个干净的250毫升单颈部圆底烧瓶. </li>
		<li> 使用旋转蒸发器除去乙醚, 并获得纯产品的11.46 克 (产量: 52.8%). </li>
	</ol>
	</li>
</ol>

<ol>
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作者没有什么可透露的。

协议中最关键的步骤是单 alkylphosphinic 酸合成 (图 1a)。在这个反应中, 较高的产量和较少的 dialkylphosphinic 酸 by-product 是更好的。增加 NaH2PO2/烯烃 A 的摩尔比将提高产量, 抑制 dialkylphosphinic 酸 by-product 的产生。但是, 大型 NaH2PO2用量也会增加成本并引起搅拌问题。NaH2PO2/烯烃 A 的首选摩尔比为3:1。作为溶剂, 呋喃是优?...

酸性有机磷萃取被广泛应用于传统的湿法冶金领域, 用于稀土离子的萃取和分离1,2, 有色金属 (如钴/镍3,4), 稀有金属 (如 Hf/锆5, V6,7), 锕8,等。近年来, 它们在二次资源回收和高级液体废物处理方面也引起了更多的关注9。二 (2-乙基己基) 磷酸 (D2EHPA 或 P204), 2-ethylhexylphosphoric 酸 mono-2-ethylhexyl 酯 (EHEHPA, PC 88A, 或 P507), 和 di (24, 4 '-2,4,4-)-膦酸 (Cyanex272), 是 dialkylphosphoric 酸的代表,alkylphosphoric 酸单烷基酯和 dialkylphosphinic 酸分别是最常用的萃取。它们的酸度按以下顺序递减: P204 和 #62; P507 和 #62; Cyanex 272。相应的萃取能力、萃取能力、剥离酸度均为 P204 和 #62; P507 和 #62; Cyanex 272, 分离性能则相反。在大多数情况下, 这三萃取是有效的。然而, 仍有一些条件, 它们不是如此有效: 在重稀土分离, 其中存在的主要问题是选择性差, 高剥离酸性 P204 和 P507, 低萃取能力, 和乳液的趋势在提取期间为 Cyanex 272。近年来, 小说萃取的发展引起了人们的广泛关注。
dialkylphosphinic 酸萃取被认为是开发新萃取的重要研究方向之一。最近的研究表明, dialkylphosphinic 酸的提取能力主要取决于烷基取代基的结构10,11。它的范围可能比 Cyanex 27212的 P507 要低得多。然而, 对新型 dialkylphosphinic 酸萃取的探索仅限于商用烯烃结构10、12、13、14、15, 16。虽然 dialkylphosphinic 酸萃取也可以通过氏反应的方法合成, 但反应条件是严格的12,17。
NSDAPA, 其中两个烷基是不同的, 打开一扇门, 探索新的萃取。它使 dialkylphosphinic 酸的结构更加多样化, 其提取和分离性能可以通过对它的烷基结构进行 fine-tuned。传统的 NSDAPA 合成方法采用 PH 值为3作为磷源, 具有毒性高、反应条件严格、不易纯化等诸多缺点。最近, 我们报告了一种新的合成 NSDAPA 的方法, 利用磷酸钠作为磷源 (参见图 1) 并成功合成了三 NSDAPAs18。这个详细的协议可以帮助新的实践者重复实验, 掌握 NSDAPA 萃取的合成方法。我们以 (23-dimethylbutyl) (24, 4 '-2,4,4-) 膦酸为例。在表 1中显示了烯烃 a、单 alkylphosphinic 酸中间体、烯烃 B 和相应的 NSDAPA 的名称和结构。

<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

本文以 (23-dimethylbutyl) (24、4-2,4,4-) 膦酸的合成为例, 说明了一种合成高纯度对称 dialkylphosphinic 酸萃取的方法。以低毒磷酸钠为磷源, 与烯烃 A (23-二甲基-1-丁烯) 发生反应, 生成 monoalkylphosphinic 酸中间体。采用金刚烷胺除去 dialkylphosphinic 酸副产品, 因为只有 monoalkylphosphinic 酸能与金刚烷胺反应形成 amantadine∙mono-alkylphosphinic 酸盐, 而 dialkylphosphinic 酸不能与金刚烷胺反应, 因为其巨大的空间位阻。纯化后的 monoalkylphosphinic 酸与烯烃 B (丁烯) 反应产生对称 dialkylphosphinic 酸 (NSDAPA)。未 monoalkylphosphinic 酸可以通过简单的碱酸后处理去除, 通过钴盐的沉淀可以分离出其他有机杂质。(23-dimethylbutyl) (24, 4 '-2,4,4-) 膦酸的结构由31P 核磁共振、 1H 核磁共振、ESI 质谱和 FT IR 证实。纯度由电位滴定法测定, 结果表明纯度可超过96%。

31用金刚烷胺法 (图 1a-b) 纯化前后的单 (23-dimethylbutyl) 膦酸的核磁共振谱。31P 核磁共振谱1H 核磁共振谱、MS 谱和 FT 红外光谱分别收集 (23-dimethylbutyl) (24、4-2,4,4-) 膦酸 (见图 3、图 4、图 5和图 6) 后用钴盐沉淀法提纯。(23-dimethy...

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

高纯度对称 Dialkylphosphinic 酸萃取的合成

介绍了一种合成高纯度对称 dialkylphosphinic 酸萃取的协议, 以 (23-dimethylbutyl) (24, 4 '-2,4,4-) 膦酸为例。

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 ...

synthesis-high-purity-nonsymmetric-dialkylphosphinic-acid

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7.4K 次观看.  University of Science and Technology Beijing. 介绍了一种合成高纯度对称 dialkylphosphinic 酸萃取的协议, 以 (23-dimethylbutyl) (24, 4 '-2,4,4-) 膦酸为例。

视频: 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.

通过中级过氧化物的抗病毒四氢咔唑衍生物的合成光化学和酸催化CH官能（筹）

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 ...

科研

化学

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.

Immunotargeted的合成磁等离子团簇

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.

的吲哚酚苷的检测糖苷酶活动的合成

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.

超分子胶体的合成与表征

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.

金纳米棒基于对苯二酚合成

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.

分层的ZnO / CdSSe异质Nanotrees的合成

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.

化学沉淀法合成铌2O5改性高比表面积镍催化剂

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.

通过活性表面生长机制合成基片束缚金纳米线

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.

[4.4] 刺环氧基的固相合成

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.

两栖金纳米粒子的合成与表征

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