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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 explore the best synthetic process of N2- (4-methylphenylsulfonyl) -L-asparagine. Methods L-asparagine and p-toluenesulfonyl chloride as raw materials, water as a solvent to explore the different acid binding agent, the reaction yield. The results of water as solvent, triethylamine as acid-binding agent, reaction at 0 ~ 5 ℃ 3 h, naturally rose to room temperature for 8 h, filtered, the mother liquor adjusted pH2, filtered to give a white solid, Rate 80.2%. Conclusion The process is stable and feasible.