HRID1977083

反应详情

EQUATION

反应方程式

HRID 1977083 的结构方程式

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

5.55 g (33.0 mmol) of 3-amino-4-cyano-1-methyl-5-methylmercaptopyrazole are heated to the boil with 50 ml of 32% strength aqueous sodium hydroxide solution for 24 hours. The reaction mixture is cooled, made slightly acidic with sodium dihydrogen phosphate solution, heated at 50° C. for 8 hours and subsequently extracted with ethyl acetate. The organic phase is dried over sodium sulfate, concentrated and purified by column chromatography (silica gel, hexane/ethyl acetate).

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled
  2. extractionsubsequently extracted with ethyl acetate
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. concentrationconcentrated
  5. custompurified by column chromatography (silica gel, hexane/ethyl acetate)