水介质中2-巯基嘧啶脱巯基的绿色合成工艺研究

Green Synthetic Technology in Dethiolation of 2-Mercaptopyrimidine

摘要:

采用中性水介质代替传统的有机溶剂，以活性Raney-Ni考察了2-巯基嘧啶脱巯基的绿色合成工艺，对含有氨基和羟基的2-巯基嘧啶的脱巯基反应条件进行优化，研究了取代基效应、反应溶剂、反应温度对Raney-Ni直接脱硫的产率影响，同时对Raney Ni及水的回收利用进行了考察，并以此制备了4-氨基-6-羟基嘧啶、4-氨基嘧啶、5,6-二氨基-4-羟基嘧啶和4-羟基嘧啶，其脱硫收率分别为98%、74%、87%及89%。该工艺反应条件为加热回流搅拌，反应时间1-4 h，可避免有机溶剂的使用，具有生产安全等优点

Abstract:

With green synthetic technology to avoid organic solvents, the aqueous medium is used to the dethiolation of 2-mercaptopyrimidine derivatives via the reduction activity of Raney-Ni. Specifically, the yield effect on the substitution, reaction solvents and temperature was optimized, along with the recycling possibility of Raney Ni and waster water. 4-Amino-6-hydroxypyrimidine, 4-aminopyrimidine, 5,6-diamino-4-hydroxypyrimidine and 4-hydroxypyrimidine were synthesized with the yields of 98%, 74%, 87% and 89%, respectively. The green synthetic process is stirred under reflux for 1-4 h, which can avoid organic solvents for improving the production safety.