曲尼司特合成工艺的改进

Improvement in Synthesis of Rizaben

采用3EA/吡啶复合溶剂,以邻氨基苯甲酸、3,4-二甲氧基肉桂酸和苯磺酰氯为原料直接合成曲尼司特。改进后的工艺,原料成本降低,合成路线缩短,产品收率提高。确定了最佳合成工艺条件:3,4-二甲氧基肉桂酸40 g,3,4-二甲氧基肉桂酸与邻氨基苯甲酸摩尔比 1.5:1,酰胺化反应温度25℃,反应时间3 h,3EA与吡啶体积比 0.03:1,吡啶用量200 mL,产品收率可达 65％。

Rizaben was synthesized directly from anthranilic acid ,3,4- dimethoxy cinnamic acid, and benzene sulfochloride using 3EA/pyridine as compounded solvent. The improved synthesis has low raw material cost, short synthetic route, and high yield of rizaben. The optimum conditions of synthesis were determined as follows: 3,4 -dimethoxy cinnamic acid 40 g, molar ratio of 3,4 - dimethoxy cinnamic acid to anthranilic acid 1.5:1, amidation temperature 25 ℃ , amidation time 3 h, volume ratio of 3EA to pyridine 0.03:1, amount of pyridine 200 mL. The yield of rizaben was up to 65 % .