CN104151545A - 一种聚乙二醇单甲醚膦配体的合成 - Google Patents
一种聚乙二醇单甲醚膦配体的合成 Download PDFInfo
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Abstract
一种聚乙二醇单甲醚膦配体的合成，包括：取10g二苯基氯化磷置于三口烧瓶中，加入V(四氢呋喃)∶V(三乙胺)=3∶1的混合溶液20mL将其溶解，于0℃时开始滴加溶解在50mL四氢呋喃中的0.75倍摩尔数的聚乙二醇单甲醚溶液，滴加完毕后保温反应6h，室温过夜，过滤后滤液经减压脱出溶剂得到白色蜡状固态产物。
Description
技术领域
本发明涉及一种聚乙二醇单甲醚膦配体的合成，属于合成化学领域。
背景技术
温控相转移催化过程是基于温控膦配体与过渡金属形成的络合催化剂的温控相转移功能，即在低(室)温下具有良好的水溶性，当温度升至浊点温度时会从水中析出并转移至有机相，因而，在反应开始前催化剂与底物分处于两相，而在高于浊点的反应温度下，催化剂从水中析出，转移至有机相和底物共处于有机相，反应在有机相中进行，待反应结束冷却至浊点以下温度时，催化剂又恢复水溶性，从有机相重返水相，从而使留在水相中的催化剂可以通过简单的相分离与含有产物的有机相分开，达到催化剂易于分离回收的目的。
发明内容
本发明提供一种聚乙二醇单甲醚膦配体的合成，包括：取10 g二苯基氯化磷置于三口烧瓶中，加入V(四氢呋喃):V(三乙胺)=3：1的混合溶液20mL将其溶解，于0 ℃时开始滴加溶解在50 mL四氢呋喃中的0.75倍摩尔数的聚乙二醇单甲醚溶液，滴加完毕后保温反应6 h，室温过夜，过滤后滤液经减压脱出溶剂得到白色蜡状固态产物。
本发明的有益效果是：膦配体与贵金属配合形成催化剂，催化反应完成后，下层催化剂相可以循环使用，从而节约了成本。
具体实施方式
以下对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。
实施例1
取10 g二苯基氯化磷置于三口烧瓶中，加入V(四氢呋喃):V(三乙胺)=3：1的混合溶液20mL将其溶解，于0 ℃时开始滴加溶解在50 mL四氢呋喃中的0.75倍摩尔数的聚乙二醇单甲醚溶液，滴加完毕后保温反应6 h，室温过夜，过滤后滤液经减压脱出溶剂得到白色蜡状固态产物8克。
实施例2
取12 g二苯基氯化磷置于三口烧瓶中，加入V(四氢呋喃):V(三乙胺)=3：1的混合溶液20mL将其溶解，于0 ℃时开始滴加溶解在50 mL四氢呋喃中的0.75倍摩尔数的聚乙二醇单甲醚溶液，滴加完毕后保温反应6 h，室温过夜，过滤后滤液经减压脱出溶剂得到白色蜡状固态产物10克。
实施例3
取10 g二苯基氯化磷置于三口烧瓶中，加入V(四氢呋喃):V(三乙胺)=3：1的混合溶液20mL将其溶解，于0 ℃时开始滴加溶解在50 mL四氢呋喃中的0.8倍摩尔数的聚乙二醇单甲醚溶液，滴加完毕后保温反应6 h，室温过夜，过滤后滤液经减压脱出溶剂得到白色蜡状固态产物8.5克。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (2)
1.一种聚乙二醇单甲醚膦配体的合成，包括：取10 g二苯基氯化磷置于三口烧瓶中，加入V(四氢呋喃):V(三乙胺)=3：1的混合溶液20mL将其溶解，于0 ℃时开始滴加溶解在50 mL四氢呋喃中的0.75倍摩尔数的聚乙二醇单甲醚溶液，滴加完毕后保温反应6 h，室温过夜，过滤后滤液经减压脱出溶剂得到白色蜡状固态产物。
2.权利要求1所述一种聚乙二醇单甲醚膦配体的合成，反应温度为零度，冰水浴保持。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110124732A (zh) * | 2019-04-13 | 2019-08-16 | 复旦大学 | 用于金属催化偶联反应的高分子催化剂及其制备方法 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124732A (zh) * | 2019-04-13 | 2019-08-16 | 复旦大学 | 用于金属催化偶联反应的高分子催化剂及其制备方法 |
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