HRID1358969
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 160 °C
PROCEDURE
实验过程
A suspension of 2-chloro-3-bromo-6-aminopyrazine (15 g, 0.072 mole) in absolute ethanol (150 ml) and 0.880 ammonia (375 ml) was stirred and heated in an autoclave at 160° C. and 20 atm. for 16 hrs The cooled mixture was evaporated in vacuo and extracted with hot methanol (3×100 ml). The combined methanol extracts were evaporated in vacuo. The residue was dissolved in hot chloroform, dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated in vacuo. The residue was triturated with 40-60° C. petroleum ether, filtered, and dried in vacuo. Yield 5.51 g (40%), M.p. 176-178° C.
WORKUP
后处理
- custom20 atm. for 16 hrs The cooled mixture was evaporated in vacuo
- extractionextracted with hot methanol (3×100 ml)
- customThe combined methanol extracts were evaporated in vacuo
- dissolutionThe residue was dissolved in hot chloroform
- dry with materialdried over anhydrous magnesium sulphate
- filtrationfiltered
- customthe filtrate evaporated in vacuo
- customThe residue was triturated with 40-60° C. petroleum ether
- filtrationfiltered
- customdried in vacuo