D-青霉胺酰化消旋工艺及动力学研究

目的研究D-青霉胺在酸性条件下进行酰化外消旋的工艺。方法以D-青霉胺为原料,在醋酸溶液中,用乙酰氯为酰化试剂进行消旋化,得到了D-青霉胺酰化消旋物;并以溶剂量、反应温度、反应时间、乙酰氯的量等为因素考察最佳工艺条件;测定反应温度、时间与消旋过程比旋度的关系,计算酰化过程的动力学方程。结果得到最佳工艺条件即青霉胺量-醋酸量-乙酰氯量(1∶7∶2),反应温度80℃,反应时间5h。酰化过程的动力学方程符合一级线性关系。结论该工艺条件缓和,路线简单,为D,L-青霉胺的制备提供了直接原料。

Acetylized Racemization Process and Kinetics of D- penicillamine

OBJECTIVE:To study the process of acetylized racemization of D-penicillamine in the acidic condition. METHODS:The acetylized racemic mixture of D-penicillamine was prepared by racemizing acetyl chloride in acetic acid solu_tion with D-penicillamine as feedstock.The preparation process was optimized with the quantities of solvent and acetyl chloride,the reaction temperature,the reaction time etc.as parameters.The influence of reaction temperature,reaction time on the specific optical rotation in the acetylized process was determined and the kinetic equation of acylation process was computed. RESULTS:The optimal condition for racemization was the following,the quantity ratios of D-penicillamine-acetic acid -acetyl chloride were 1∶7∶2,the reaction temperature was 80℃ and the reaction time was 5h.The kinetic equation of acylation process fitted first order linear relation. CONCLUSION:This preparation process is mild and simple,and it offers direct feedstock for the preparation of D,L-penicillamine.