邻氯苯甘氨酸甲酯的绿色合成工艺研究

Environmental-friendly Synthesis of 2-chlorophenylglycine Methyl Ester

以邻氯苯甘氨酸为原料,在乙酰氯与甲醇制成的氯化氢甲醇溶液中,进行原位氯化氢催化酯化,绿色合成了标题化合物。通过正交实验研究各因素(物料比、反应温度、反应时间)对产率的影响,找到了最佳合成工艺条件。该反应最佳工艺条件是:物料比为1∶3,反应温度为45℃,反应时间为10 h,收率高达95.6%。与文献相比,该反应条件温和,环境友好,收率较高。目标产物通过MS和1H NMR进行了结构表征。

The target compound was environmental-friendly synthesized by in-situ hydrogen chloride catalysis based on 2-chlorophenylglycine as raw material,in the methanol solution of hydrogen chloride prepared by acetyl chloride and methanol.Meanwhile,the effect of factors（material ratio,reaction temperature,reaction time） on the yield were studied by orthogonal experiments,and the optimum synthesis condition was found.The optimum reaction condition was material ratio of 1 ∶ 3,reaction temperature of 45 ℃,reaction time of 10 h,with a highest yield of 95.6%.Compared with the literature,the synthesis process was mild,environmental-friendly and with a higher yield.Moreover,the structure of the product was confirmed via MS and1 H NMR.