3-氯-L-丙氨酸盐酸盐的合成研究

Study on the Synthesis of 3-chlorine-L-alanine Hydrochloride

通过对反应过程的优化,探索3-氯-L-丙氨酸盐酸盐的最佳合成工艺并对中间产物以及最终产物进行质谱表征。实验得最佳工艺为:5.00 g的L-丝氨酸和4.15 ml二氯亚砜,低温反应1 h后升温至40℃继续反应4.5 h,产率约83.9%;5.00 g的L-丝氨酸甲酯盐酸盐和7.36 g五氯化磷,冰水浴下反应2 h后升温至30℃继续反应2 h,产率约95.3%;5.00 g的3-氯-L-丙氨酸甲酯盐酸盐在50 mL的6 mol/L的盐酸中先回流反应1 h后再蒸馏反应0.8 h,产率约75.4%。总产率约60.3%。

By optimizing the three-step reaction,the optimum synthesis process of 3-chloro-l-alanine hydrochloride was explored and the intermediate and final products were characterized by mass spectrometry.The optimal process was obtained as follows:5 g L-serine and 4.15 ml dichlorosulfoxide were reacted at low temperature for 1 h and then heated to 40℃ for 4.5 h,with a yield of about 83.9%.5 g of L-serine methyl ester hydrochloride and 7.36 g of phosphorus pentachloride were reacted in ice water bath for 2 h and then heated to 30℃ for 2 h,with a yield of about 95.3%.5 g 3-chloro-l-alanine methyl ester hydrochloride was reflux reaction for 1 hour and then distillation reaction for 0.8 hour in 50 ml 6 mol/L hydrochloric acid,with a yield of about 75.4%.The total yield was about 60.3%.