苯酞-3-羧酸合成工艺的改进  

Improved Synthesis of Phthalide-3-carboxylic Acid

作　　者：冯德日 汪亚伦[1] 师秀艳[1] 

机构地区：[1]沈阳医学院,辽宁沈阳110034

出　　处：《精细化工》2014年第6期784-787,共4页Fine Chemicals

基　　金：沈阳医学院科技基金项目(20122035)~~

摘　　要：该文以邻苯二甲酸酐为原料,经硼氢化钠还原,在六甲基二硅基氨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。考察了还原反应还原剂用量、反应时间、反应温度,缩合反应的投料比、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%,终产品纯度为96.8%,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。In this study, phthalic anhydride was reduced by sodium borohydrid, then condensed with ethyl chloroformate under the effect of KHMDS, and the product of the condensation was then hydrolyzed to give the phthalide-3-carboxyiic acid which was the final target compound. The effects of reducing agent proportion, reaction time and reaction temperature 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 64.2%, and the purity of product was 96.8%. The reaction conditions were mild, in which the use of sodium cyanide ,which was violent in toxicity,was avoided. The structure of the target compound was confirmed by means of ESI- MS and 1HNMR.

关 键 词：苯肽-3-羧酸 邻苯二甲酸酐 工艺研究 精细化工中间体 

分 类 号：TQ463[化学工程—制药化工]