除草剂乙氧呋草黄的合成与表征

Synthesis and Characterization of Herbicidal Ethofumesate

通过吗啉和异丁醛合成烯胺 ,然后与对苯醌缩合成环 ,经甲基磺酰氯以及乙醇反应 ,合成了烯胺、2 - (4’ -吗啉基 ) - 2 ,3-二氢化 - 3,3-二甲基 - 5-苯并呋喃酚、2 - (4’ -吗啉基 ) - 2 ,3-二氢化 - 3,3-二甲基 - 5-苯并呋喃基甲基磺酸酯、2 -乙氧基 - 2 ,3-二氢化 - 3,3-二甲基 - 5-苯并呋喃基甲基磺酸酯 (乙氧呋草黄 )。通过红外光谱、核磁共振验证了各中间体结构 ,高效液相色谱测试了其纯度 ,测定了相应熔点。通过实验 ,找到了较佳的合成条件 ,平均得率为 79.2 %。

ethoxy-2,3-dihydro-3,3-dimethyl-benzofuran-5-yl methanesulfonate (ethofumesate) was prepared by treating isobutyraldehyde with morpholine , condensing the enamine with benzoquinone, and treating 2- morpholino-2,3-dihydro-3,3-dimethyl-benzofuran-5-ol with methanesulfonylchloride and alcohol. The structure of samples was characterized by infrared spectroscopy and nuclear magnetic resonance;and the purity of ethofumesate was measured by high performance liquid chromatography; the melting point of the samples was measured at the same time. The results show that the yield of ethofumesate was 79.2% in the optimum synthesis condition.