7-苯乙酰氨基-3-乙烯基头孢烷酸对甲氧苄酯的合成工艺研究

Synthetic process study on 7-phenylacetamido-3-vinyl carboxylic acid p-methoxybenzyl ester

选用7-苯乙酰氨基-3-氯甲基头孢烷酸对甲氧苄酯(GCLE)为原料制备了7-苯乙酰氨基-3-乙烯基头孢烷酸对甲氧苄酯。GCLE与卤化物、三苯基膦反应生成3位膦盐,在碱性条件下得到Wittig试剂(膦叶立德),再与甲醛反应生成7-苯乙酰氨基-3-乙烯基头孢烷酸对甲氧苄酯。实验结果采用正交表进行分析,结果表明,选用KI为卤化剂,K2CO3为碱性介质,n(甲醛)∶n(GCLE)为1∶10,溶剂为丙酮/CH2Cl2时,所得产物收率较高。

GCLE was selected as raw material to prepare 7-phenylacetamido-3-vinyl carboxylic acid p-methoxybenzyl ester.The process was as follows：GCLE was reacted with iodide in solvent,and 3-iodid was given,which was reacted with PPh3 to produce Wittig agent,and Wittig agent was reacted with HCHO to produce 7-phenylacetamido-3-vinyl carboxylic acid p-methoxybenzyl ester in alkaline condition.In according to the analysis of orthogonal table,the conclusions were obtained：KI as iodide,K2CO3 as alkaline solution,the formaldehyde dosage as 1∶10,and acetone and CH2Cl2 as solvents,the productive rate was high.