A Study on the Synthesis Method of Phenylpeptidylamine Acid
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%.
phenylpeptidylamine acidsynthesis methodammoniolysishydrolysiscatalystsreaction temperature and timeboosteryield