HRID1869402

反应详情

EQUATION

反应方程式

HRID 1869402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution that consists of 5-chloro-4-nitro-1H-indazole (872 mg, 4.41 mmol) is mixed with 150 mg of palladium on carbon (10%) and stirred under hydrogen atmosphere at room temperature. After 45 minutes, the catalyst is suctioned off on one frit and washed with methanol. The filtrate is concentrated by evaporation, and the residue is taken up in 200 ml of ethyl acetate and heated. After renewed suctioning-off and concentration by evaporation of the filtrate, the purification on silica gel is carried out with hexane/ethyl acetate (100-33% hexane). 296 mg (40% of theory) of the product is obtained.

WORKUP

后处理

  1. washwashed with methanol
  2. concentrationThe filtrate is concentrated by evaporation
  3. temperatureheated
  4. concentrationconcentration
  5. customby evaporation of the filtrate
  6. customthe purification on silica gel
  7. custom296 mg (40% of theory) of the product is obtained