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以邻苯二乙醚为主要原料,经混酸硝化后催化加氢还原,得中间体对氨基邻苯二乙醚,再与氯甲酸异丙酯缩合,得到乙霉威。结果表明,催化加氢还原的最佳条件:反应温度90℃,催化剂用量为反应物质量的3%,压力1.5 MPa,反应时间3 h;缩合反应的最佳条件:以三乙胺为缚酸剂,溶剂甲苯与反应物的质量比为2.1∶1,对氨基邻苯二乙醚与氯甲酸异丙酯的摩尔比为1∶1.3,反应时间0.5 h。在较佳的反应条件下,乙霉威的总收率≥80.38%,含量≥98%。
With o-diethyl ether as the main raw material, the mixed acid nitration after catalytic hydrogenation, the intermediate of amino-ortho-diethyl ether, and then with isopropyl chloroformate to give diethofen. The results showed that the optimal conditions for the catalytic hydrogenation were: the reaction temperature was 90 ℃, the amount of catalyst was 3% of the reactant, the pressure was 1.5 MPa and the reaction time was 3 h. The optimal conditions for the condensation reaction were triethylamine The mass ratio of solvent to toluene was 2.1: 1, the molar ratio of p-aminophenyl ether and isopropyl chloroformate was 1: 1.3, and the reaction time was 0.5 h. Under the best reaction conditions, the total yield of diethofencarb was ≥80.38% and the content was ≥98%.