HRID2379884

反应详情

EQUATION

反应方程式

HRID 2379884 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureunder refluxing for 20 minutes
  2. temperatureThe mixture was refluxed for 4 hours
  3. customThe solvent was removed under reduced pressure
  4. dissolutionthe residue was dissolved in water (100 ml)
  5. extractionThe mixture was extracted with a mixture of ethyl acetate (300 ml) and tetrahydrofuran (150 ml)
  6. dry with materialThe extract was dried with magnesium acetate
  7. customevaporated