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[求助]
锰卟啉的合成
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请教下如何除去锰卟啉合成过程中的四丁基氯化铵？？ 实验条件如下：Metallation in methanol was accomplished under refluxing conditions, whereas in water it was achieved at room temperature. Routinely, a 1:20 ratio of porphyrin to metal in water at room temperature was applied. The reaction was monitored by UV-visible spectroscopy. Upon completion of metallation (pH brought to ～7), the solution was filtered to remove manganese hydroxo species, and the PF6− salt of manganese complex was precipitated by the addition of a concentrated aqueous solution of NH4PF6. The compound was then dissolved in acetone, the solution was filtered, and a concentrated acetone solution of tetrabutylammonium chloride was added, until the majority of the porphyrin had precipitated in the form of its chloride salt. 紫外表征显示反应成功，但实验过程中有两个问题，第一是加入高浓度的四丁铵氯化铵丙酮溶液后，没有产生沉淀，但刚加入后溶液的颜色就发生很明显的变化，多加颜色不会改变，推测生成了氯盐。第二个是由于锰卟啉不能沉降，尝试用良溶剂和惰性溶剂的方法分离，但发现四丁铵氯化铵能够溶于多数溶液中，很难将其分离。目前没有办法去除掉四丁铵氯化铵，求教。 |
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