不对称转化法制备D-苯甘氨酸

Preparation of D-phenylglycine by asymmetric resolution

目的拆分外消旋苯甘氨酸得到D-苯甘氨酸。方法以d-樟脑-10磺酸为拆分剂,水杨醛为催化剂,在冰醋酸溶剂中拆分外消旋苯甘氨酸得到D-苯甘氨酸。结果与结论讨论了原料配比、反应温度、反应时间和催化剂用量对反应结果的影响,确定了制备D-苯甘氨酸酒石酸盐的最佳工艺条件为n(外消旋苯甘氨酸)∶n(d-樟脑-10磺酸)∶n(水杨醛)=1.00∶1.05∶0.02,反应温度为80℃,反应时间为5 h。D-PG.d-CS盐用氨水碱化,经等电点法提纯后得D-PG,总收率质量分数为78.9%,光学纯度为99.7%ee。

Objective To prepare D-phenylglycine by asymmetric resolution of DL- phenylglycine. Method The experiment was performed with d-camphor-10-sulfonic acid as resolution agent in acetic acid using salicyladehyde as catalyst. Result and conclusion The influences of reagent molar ratio, time, temperature and catalyst dosage were discussed. The overall yield was 78.9 % with. the optical purity of 99.7 %.