2,3-二氢-1,5-苯并噻庚因-4(5H)-酮及其衍生物合成方法的改进  

A Modified Method for Synthesis of 2,3-Dihydro-1,5-benzothiazepin-4(5H)-one and Their Derivatives

作　　者：陈勇[1] 张新兵[1] 

机构地区：[1]江苏工业学院化学工程系,江苏常州213016

出　　处：《农药》2007年第3期159-161,共3页Agrochemicals

摘　　要：邻氨基硫酚在邻、对氯甲苯溶剂中分别与丙烯酸、肉桂酸、呋喃丙烯酸反应得到相应的2,3-二氢-1,5-苯并噻庚因-4(5H)-酮及其衍生物(Ia～c),收率分别为87.6%、76.3%和69.5%。用红外光谱、核磁共振光谱、质谱对产物进行了分析,证明所得产物为目标化合物。研究了2,3-二氢-1,5-苯并噻庚因-4(5H)-酮(Ia)的合成,其优化条件为:n(酚)∶n(酸)为1∶1,溶剂用量为70mL,加料时反应温度为100℃,加料时间为60min,然后将反应温度升至反应混合物沸点,并将反应过程中产生的水及时去除。2,3-Dihydro-1,5-benzothiazepin-4（5H）-ones and their derivatives（Ia-c） were prepared by reaction of 2-aminothiophenol with acrylic acid and substituted acrylic acids in the presence of chlorotoluene mixture as solvent, respectively, in 87.6%, 76.3% and 69.5% yield. Their structures were characterized by IR, 1H NMR and MS. Synthesis of Ia were studied emphatically. The best technological conditions were： n（phenol）：n（acid）=1：1, the amount of solvent 70 mL, the feed temperature 100 ℃, the feed time 60 min. After that the temperature was increased to the boiling point of the reaction mixture and the water was removed by azeotropic distillation.

关 键 词：邻氨基硫酚 2 3.二氢-1 5-苯并噻庚因-4(5H)-酮 合成 

分 类 号：TQ450.2[化学工程—农药化工]