HRID652092

反应详情

EQUATION

反应方程式

HRID 652092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of 3-bromo-5-nitro-1H-1,2,4-triazole (13.1 g) in acetone (100 ml) was cooled to 0° and treated with 10% sodium hydroxide solution (30 ml), followed by dimethyl sulphate (9.5 g). After 18 h at room temperature, the mixture was evaporated in vacuo; the residue was diluted with water and extracted with ethyl acetate. The combined extracts were washed with 2N sodium hydroxide solution, water, and evaporated in vacuo. The resulting solid was recrystallized from a mixture of ethyl acetate and cyclohexane to yield the title compound (6.0 g), m.p. 90.5°-91.5°.

WORKUP

后处理

  1. customthe mixture was evaporated in vacuo
  2. additionthe residue was diluted with water
  3. extractionextracted with ethyl acetate
  4. washThe combined extracts were washed with 2N sodium hydroxide solution, water
  5. customevaporated in vacuo
  6. customThe resulting solid was recrystallized from a mixture of ethyl acetate and cyclohexane