HRID2379884
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
PROCEDURE
实验过程
A solution of sodium borohydride (1.2 g) in water (25 ml) was added slowly to a solution of 2-(diaminomethyleneamino)-4-(5-methoxycarbonylpyridin-3-yl)thiazole (2.8 g) in methanol (70 ml) and tetrahydrofuran (70 ml) under refluxing for 20 minutes. The mixture was refluxed for 4 hours. The solvent was removed under reduced pressure and the residue was dissolved in water (100 ml). The mixture was extracted with a mixture of ethyl acetate (300 ml) and tetrahydrofuran (150 ml). The extract was dried with magnesium acetate and then evaporated to afford 2-(diaminomethyleneamino)-4-(5-hydroxymethylpyridin-3-yl)thiazole (1.14 g).
WORKUP
后处理
- temperatureunder refluxing for 20 minutes
- temperatureThe mixture was refluxed for 4 hours
- customThe solvent was removed under reduced pressure
- dissolutionthe residue was dissolved in water (100 ml)
- extractionThe mixture was extracted with a mixture of ethyl acetate (300 ml) and tetrahydrofuran (150 ml)
- dry with materialThe extract was dried with magnesium acetate
- customevaporated