HRID1292965

反应详情

EQUATION

反应方程式

HRID 1292965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 5-nitroindazole (10.0 g, 61.3 mmol) in acetonitrile (100 mL) was added potassium carbonate (16.9 g, 122.6 mmol) and benzyl bromide (13.6 g, 79.7 mmol). The resulting yellow reaction mixture was heated with stirring at 70° C. overnight. Upon cooling down, the solid was filtered off and washed with methylene chloride. The filtrate was concentrated to dryness and the resulting residue was purified by flash chromatography eluting with 17–25% ethyl acetate in hexanes (v/v) yielding 7.0 g (44%) of the corresponding 1-Benzyl-5-nitro-1H-indazole as a yellow solid.

WORKUP

后处理

  1. temperatureThe resulting yellow reaction mixture was heated
  2. temperatureUpon cooling down
  3. filtrationthe solid was filtered off
  4. washwashed with methylene chloride
  5. concentrationThe filtrate was concentrated to dryness
  6. customthe resulting residue was purified by flash chromatography
  7. washeluting with 17–25% ethyl acetate in hexanes (v/v)