不对称转换法制备D-脯氨酸的工艺研究

Study on the Synthesis of D-Proline by Asymmetric Transformation

以L-脯氨酸(L-Pro)为原料,正丁醛作催化剂,在正丁酸溶剂中,与R-酒石酸(R-TA)反应制备D-Pro.R-TA.着重研究了反应温度、反应时间、羧酸溶剂用量和催化剂的用量对产物收率和光学纯度的影响,获得了最佳工艺条件.即:反应温度为90℃,反应时间为6 h,正丁酸为溶剂(60 mL),n(L-Pro)∶n(R-TA)∶n(正丁醛)=1∶1∶0.1(mol),中间体D-Pro-R-TA在甲醇中加35%的氨水处理得到D-脯氨酸,总收率为91.74%,光学纯度为98.7%.

D-Pro·R-TA salt was obtained through the reaction of L-Pro with R-TA in n-Butyric acid with butyl aldehyde as catalyst. The influences of temperature, time, carboxylic acid dosage and catalyst dosage on the yield and optical purity were discussed . The optimal process conditions are as follows： reaction temperature 90℃, reaction time 6h, n-Butyric acid as solvent （60 mL） and L-Pro： R-TA： butyl aldehyde = 1：1 ： 0.1 （tool）. Treatment of the obtained salt D-Pro·R-TA with 35% ammonia in methanol gare D-Pro is obtained with the yield of 91.74% and the optical purity of 98, 7% based on the starting L-Pro.