作　　者： ; ; ;

机构地区： 暨南大学生命科学技术学院化学系

出　　处： 《有机化学》 2005年第9期1125-1128,共4页

摘　　要： 经氟代、水解脱羧、酯化、还原等步骤合成了杀虫剂四氟苯菊酯的重要中间体2,3,5,6-四氟苯甲醇,改进了氟代反应的无水操作和反应条件,产物四氟对苯二甲腈纯度高达98.3%,通过加入水参与反应改进了水解反应,使水解和脱羧由两步反应变为一步,且产物为只脱一个羧基的2,3,5,6-四氟苯甲酸,收率可以高达92.5%,用相对价廉的NaBH4/I2体系还原2,3,5,6-四氟苯甲酸甲酯以52.3%的收率得到了目标产物,总收率29.6%. 2,3,5,6-Tetrafluorobenzyl alcohol, the important intermediate of insecticide transfluthrin, was synthesized through fluorination, hydrolysis, decarboxylation, esterification and reduction. Using anhydrous DMF in fluorination step, the yield of tetrafluoro-terephthalonitrile could be improved to 70.3%, with purity of 98.3%. The hydrolysis and decarboxylation occurred in one step by addition of water, and the yield of product 2,3,5,6-tetrafluorobenzoic acid was 92.5%. 2,3,5,6-Tetrafluorobenzyl alcohol was yielded with 52.3% by reduction of methyl 2,3,5,6-tetrafluorobenzoate with NaBH4/I2. Total yield was 29.6%.

关 键 词： 四氟苯甲醇 四氟苯甲酸 合成 还原 苯甲醇 水解反应 反应条件 氟代反应 苯甲酸甲酯 总收率

领　　域： [化学工程] [化学工程]