HRID127189

反应详情

EQUATION

反应方程式

HRID 127189 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a refluxing solution of 6-chloro-2,4-diaminopyrimidine (4.0 g) in anhydrous methanol (40 ml) was added methylhydrazine (3.2 g). After 18 hours the refluxing mixture was allowed to cool to room temperature under a nitrogen atmosphere in order that the product could crystallise out. The white solid (3.0 g) was collected by filtration and dried under reduced pressure at 70° C. Recrystallisation of the product from methanol/methylhydrazine (50/l) gave straw-coloured crystals of 2,4-diamino-6-(1-methylhydrazino)pyrimidine (1.92 g; 56% of theoretical yield; M.P. 214°-217° C. decomposition).

WORKUP

后处理

  1. customcould crystallise out
  2. filtrationThe white solid (3.0 g) was collected by filtration
  3. customdried under reduced pressure at 70° C
  4. customRecrystallisation of the product from methanol/methylhydrazine (50/l)