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目的改进减肥药新利司他的合成工艺。方法以2-氨基-5-甲基苯甲酸为起始原料,经甲酯化、与氯甲酸十六烷基酯缩合、再脱除甲酯保护、使用氯甲酸乙酯进行环合制得新利司他。结果与结论目标化合物的结构经~1H-NMR和MS谱确证,总收率为65%(以2-氨基-5-甲基苯甲酸计),纯度为99.8%(HPLC法)。改进后的工艺无需色谱纯化,避免使用高毒、昂贵催化剂,更适宜工业化生产。
Objective To improve his synthesis process of diet pills Novartis. Methods Starting from 2-amino-5-methylbenzoic acid, methyl esterification, condensation with cetyl chloroformate, and then the protection of methyl ester were removed and cyclopropyl was synthesized using ethyl chloroformate Listiot him. Results and Conclusions The structure of the target compound was confirmed by ~ 1H-NMR and MS spectra. The overall yield was 65% (based on 2-amino-5-methylbenzoic acid) with a purity of 99.8% (HPLC method). The improved process without chromatographic purification, to avoid the use of highly toxic, expensive catalyst, more suitable for industrial production.