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.
出处
《农药》
CAS
北大核心
2007年第3期159-161,共3页
Agrochemicals
