摘要
目的探索N2-(4-甲基苯磺酰基)-L-天冬酰胺的最佳合成工艺。方法以L-天冬酰胺与对甲苯磺酰氯为原料、水为溶剂,探索不同的缚酸剂,对反应收率的影响。结果以水为溶剂、三乙胺为缚酸剂,于0～5℃反应3 h,自然升至室温反应8 h,过滤,调母液pH2,过滤得白色固体,用甲醇精制得目标物,收率80.2%。结论该工艺稳定可行。
OBJECTIVE To find out the most effective synthetic method of N2-（4-methyl phenyl） sulfonyl-L-asparagin.METHODS Using L-asparagine and toluenesulfonyl chloride as starting material,various bases as the bind acid agents.The influence on the results in water was sought out.RESULTS Et3N was the appropriate bind acid agent and the optimum reaction condution was that the mixture was stirred at 0-5 ℃ for 3 h and another 8 h at room temperature in water.Then the mixture was filtered and the filtrated was adjusted to pH2 with concentrated hydrochloric acid.Then the white solid was got and refinded with methanol to get the target compound with yield of 80.2%.CONCLUSION The procedure is stable and operative.
出处
《华西药学杂志》
CAS
CSCD
北大核心
2012年第6期618-619,共2页
West China Journal of Pharmaceutical Sciences
