4-AA生产过程中对羟基保护反应的工艺优化

Optimization of hydroxyl group protection technology in 4-AA synthesis

目的为了降低合成4-乙酰氧基氮杂环丁酮(4-AA)的成本,对羟基保护的过程进行了工艺优化。方法改变合成过程中的溶剂、碱和温度等方法,用HPLC测定反应产物的含量,摸索了最佳的反应条件。结果在25℃条件下,以咪唑为碱,NN-二甲甲酰胺为溶剂的反应效果最佳。结论实验结果表明此条件下的反应产率为98.65%,适合于工业化生产。

Objective To optimize procedure of protecting hydroxyl group to reduce the cost of 4-AA.Methods Solvent,base and temperature were changed to determine content of reaction products.Results The best condition was temperature：25 ℃;base： imidazole;solvent：DMF.Conclusion The highest yield of this reaction was 98.65%,which was suitable for industrial manufacturing.