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[方法]2,4-二甲基-3-氨基噻吩主要用于有机合成,是合成除草剂的重要中间体。以巯基乙酸和乙酰丙酮为起始原料,经过亲核加成、酯化、关环、水解、脱羧、还原等7步反应得到2,4-二甲基-3-氨基噻吩,并优化了关键的硝化反应。[结果]正交试验显示硝化反应的最优条件:反应温度15℃,3,5-二甲基噻吩-2-甲酸与乙酰硝酸酯的摩尔比1∶7,反应时间55 min。[结论]该路线简单经济,条件温和,收率高于其他路线,适合生产。
[Method] 2,4-dimethyl-3-aminothiophene is mainly used for organic synthesis and is an important intermediate of synthetic herbicides. Using thioglycolic acid and acetylacetone as starting materials, 2,4-dimethyl-3-aminothiophene was obtained through 7 steps of nucleophilic addition, esterification, ring closure, hydrolysis, decarboxylation and reduction, and the key was optimized The nitration reaction. [Result] The orthogonal experiment showed that the optimum conditions of nitrification reaction were as follows: the reaction temperature was 15 ℃, the molar ratio of 3,5-dimethylthiophene-2-carboxylic acid and acetyl nitrate was 1: 7, and the reaction time was 55 min. [Conclusion] The route is simple and economical with mild conditions, yield is higher than other routes, suitable for production.