一种苯肽胺酸合成方法的研究

A Study on the Synthesis Method of Phenylpeptidylamine Acid

对苯肽胺酸三种合成工艺路线之羧酸法、酸酐法和羧酸酯法进行研究,最终选取对羧酸酯法开展进一步研究——考察了不同因素对目标产物收率和产品中苯肽胺酸含量的影响,重点对氨解反应催化剂及其用量、催化剂与物料摩尔比、氨解反应温度和时间、水解反应时间和用水量等因素对苯肽胺酸合成的影响进行了考察,并对添加增效剂对苯肽胺酸合成的影响进行了考察。最终得到苯肽胺酸优选合成工艺条件为:氨解反应催化剂甲醇钠与苯胺和邻苯二甲酸二乙酯的摩尔比为1∶10∶10,氨解反应温度为150~160℃,氨解反应时间为2.0~2.5 h,水解反应时间为2.5~3.0 h,水解反应用水量与原料的摩尔比为(20~25)∶1。在优选工艺条件下,羧酸酯法合成苯肽胺酸工艺路线得到的产品收率在84%以上,产品纯度(产品中苯肽胺酸含量)在94%以上,产品折百收率在80%以上。

A study was conducted on the carboxylic acid method,anhydride method,and carboxylic acid ester method for the synthesis of phenylpeptidylamine acid.Finally,the carboxylic acid ester method was selected for further research.The effects of different factors on the yield of the target product and the content of phenylpeptidylamine acid in the product were investigated,with a focus on the catalytic agent and its dosage,catalyst to material molar ratio,aminolysis reaction temperature and time The effects of hydrolysis reaction time and water consumption on the synthesis of phenylpeptidic acid were investigated,and the effect of adding enhancers on the synthesis of phenylpeptidic acid was also investigated.The optimal synthesis process conditions for phenylpeptidic acid were obtained as follows:the molar ratio of methanol sodium to aniline and diethyl phthalate in the ammonolysis reaction catalyst was 1∶10∶10,the ammonolysis reaction temperature was 150-160℃,the ammonolysis reaction time was 2.0-2.5 h,the hydrolysis reaction time was 2.5-3.0 h,and the molar ratio of water consumption to raw materials in the hydrolysis reaction was(20-25)∶1.Under optimal process conditions,the yield of the product obtained by the carboxylate ester method for synthesizing phenylpeptidylamino acid is over 84%,the purity of the product(phenylpeptidylamino acid content in the product)is over 94%,and the product yield is over 80%.