苯酞-3-羧酸合成工艺的改进

Improved synthesis of phthalide-3-carboxylic acid

摘要:

本文以邻苯二甲酸酐为原料，经硼氢化钠还原，六甲基二硅基胺基钾作用下与氯甲酸乙酯缩合，最后水解，得到目标化合物苯酞-3-羧酸。并考察了还原反应还原剂的用量、反应时间，取代反应的投料比、反应时间、反应温度对反应收率的影响。优化后3步反应总收率可达64.2%，且反应条件温和避免了氰化钠等剧毒性物质的使用，产品经ESI-MS和1HNMR确证结构。

Abstract:

In this study, phthalic anhydride was reduced by sodium borohydrid,then condensed with ethyl chloroformate on the effect of KHMDS, the product of the condensation was then hydrolysesed to give the phthalide-3-carboxylic acid which was the final target compounds. The effects of reducing agent proportion and reaction time on the yield of the reduction were studied,and also the effects of reagent mole ratio,reaction temperature and reaction time on the yield of the condensation were studied.After 3 steps,the total yield could reach up to 64.2%, the reaction condition was mild, and sodium cyanide which was the violent in toxicity was avoided to use,the structure of the targer compound was confirmed by means of ESI-MS and 1HNMR.