HRID352336

反应详情

EQUATION

反应方程式

HRID 352336 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Approximately 400 mg of Raney nickel is added to a mixture of 3.28 g (15.9 mmol) of 5-nitro-1-propylindoline and 4 ml (80 mmol) of hydrazine hydrate in 60 ml of absolute ethanol. The reaction mixture is heated under reflux for 5 hours. After returning to 23° C., a little silica is added to the flask and the solvent is evaporated off under vacuum. The evaporation residue is placed directly at the top of a chromatography column. The expected product is eluted using a Heptane/AcOEt mixture (1/9). A black oil is obtained which is used directly in the following stage.

WORKUP

后处理

  1. temperatureThe reaction mixture is heated
  2. temperatureunder reflux for 5 hours
  3. customAfter returning to 23° C.
  4. additiona little silica is added to the flask
  5. customthe solvent is evaporated off under vacuum
  6. washThe expected product is eluted
  7. customA black oil is obtained which