有点长，先谢谢各位阅读，欢迎各种讨论回答。
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我已经得到纯净的原料，反应也有产物，但是得到的不是沉淀而是粘稠物。
主要疑问有以下几点：
1.反应物是一个内盐，溶解度很差。用乙腈作溶剂，形成的是乳白色的液体（有明显的不溶颗粒），加入酰氯反应一段时间溶液变澄清。我推测是反应生成的氯化氢作为反离子，消解了内盐结构。想问一下原文献中反应接束后的filtered是为什么，是我的反应不对还是理解有误。我不想在反应中引入反离子，有什么方法或还能用什么溶剂。
2.反应要不要加三乙胺之类的缚酸剂，我在实验中有加入与醇等摩尔量的三乙胺（本以为原文中的filtered是滤的三乙胺盐酸盐，但是反应结束没有盐析出，蒸掉乙腈，换成氯仿后有盐析出）。
3.氯仿溶液水洗的时候形成乳液，很难破乳，有什么方法避免或解决。
4.re-precipitating是什么操作。是用乙醚做沉淀剂，将分液干燥后的氯仿溶液滴加到过量的乙醚中吗？
文献中的合成步骤：
Acryloyl chloride (0.3 mol) was slowly added to a magnetically stirred solution of 3-((11-hydroxyundecyl)-imidazolyl) propyl sulfonate (0.1 mol) in dried acetonitrile (200 ml) at 0[deg.] C. purged with N2 gas. The mixture was further reacted at room temperature for 3 days. The mixture was filtered and the excess acryloyl chloride and acetonitrile were removed in a rotary evaporator. The residue was dissolved in distilled chloroform, washed twice with saturated sodium bicarbonate solution followed by saturated brine and left to dry overnight by magnesium sulfate. The pure product of 3-((11-acryloyloxyundecyl)-imidazolyl) propyl sulfonate was obtained by re-precipitating the crude product  in anhydrous ether. The precipitate was filtered and dried in a vacuum oven.
新人问题有点多，金币不多，各位大神见谅。

[ Last edited by 姜小白· on 2013-3-18 at 21:10 ]

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