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机构地区:[1]华东理工大学精细化工研究所,上海200237 [2]华东理工大学科技信息研究所,上海200237
出 处:《精细化工》2013年第10期1194-1197,共4页Fine Chemicals
基 金:国家自然科学基金(21176075)~~
摘 要:采用中性水介质代替传统的有机溶剂,以活性RaneyNi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RaneyNi直接脱硫收率的影响,同时对RaneyNi及水的回收利用进行了考察,并以此制备了4-羟基嘧啶、4-氨基嘧啶、4-氨基-6-羟基嘧啶和4,5-二氨基-6-羟基嘧啶,其脱硫收率分别为98%、74%、87%及89%。该工艺条件为加热回流搅拌,反应时间1~4h,可避免有机溶剂的使用,具有生产安全等优点。With green synthetic technology to avoid organic solvents, the aqueous medium was used in the dethiolation of 2-mercaptopyrimidine derivatives via the reduction activity of Raney Ni. Specifically, the reaction conditions were optimized and the effect on the product yield of the substitution, reaction solvents and temperature was investigated, along with the recycling possibility of Raney Ni and waster water. 4-Hydroxypyrimidine, 4-aminopyrimidine, 4-amino-6-hydroxypyrimidine and 4, 5-diamino-6- hydroxypyrimidine were synthesized with yields of 98% ,74% ,87% and 89%, respectively. The green synthetic process involves a stir under reflux for 1 - 4 h and avoids the use of organic solvents, hence the improved production safety.
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