除草剂乙氧呋草黄的合成

摘要

Ethofumesate was synthesized with morpholine, isobutyraldehyde, pbenzoquinone, 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.%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20～45 ℃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30～40 ℃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10 h。经此条件下的放大实验,平均收率79.2%,纯度大于98%。