除草剂乙氧呋草黄的合成

SYNTHESIS OF HERBICIDE ETHOFUMESATE

以吗啉、异丁醛、对苯醌、甲基磺酰氯和乙醇为原料 ,经烯胺 A、中间体 B、中间体 C的制备 ,合成了乙氧呋草黄 ,纯度 99.3 % ,溶点 66.7～ 67.0℃。实验得到的较佳合成条件是 :合成 B的物料摩尔比为异丁醛∶吗啉∶对苯醌 =2 .1∶ 1∶ 1 ,在 2 0～ 4 5℃反应 3 h。从 B合成 C物料摩尔比为 B∶甲基磺酰氯∶三乙胺 =1∶ 2∶ 4 ,在 3 0～ 4 0℃反应 2 h。从 C合成乙氧呋草黄的物料摩尔比为 C∶乙醇∶盐酸 =1∶ 4∶ 2 ,在室温下反应 1 0 h。经此条件下的放大实验 ,平均收率 79.2 % ,纯度大于 98%

Ethofumesate was synthesized with morpholine, isobutyraldehyde, pbenzoquinone, mathyl sulfonylchloride and alcohol. Its construction was identified by NMR, its purity was analyzed by HPLC, and its melting point was examined. The better synthesis conditions by a serial of tests were summarized.