HRID1269880

反应详情

EQUATION

反应方程式

HRID 1269880 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 1-(methylsulfonyl)-5-nitro-1H-indazole (1.00 g, 4.15 mmol) in ethanol (20 ml) were added 10% Pd-C (100 mg) and then ammonium formate (1.57 g, 24.9 mmol), and the resulting mixture was heated under reflux for 1 hour. The solid was removed by filtration using Celite, and the solvent was distilled off under reduced pressure. Ethyl acetate/water was added to the residue, followed by extraction with ethyl acetate, and the extract solution was washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate, and then distilled under reduced pressure to remove the solvent, whereby 1-(methylsulfonyl)-1H-indazol-5-amine (425 mg, 49%) was obtained.

WORKUP

后处理

  1. temperatureunder reflux for 1 hour
  2. customThe solid was removed by filtration
  3. distillationthe solvent was distilled off under reduced pressure
  4. additionEthyl acetate/water was added to the residue
  5. extractionfollowed by extraction with ethyl acetate
  6. washthe extract solution was washed with a saturated aqueous sodium chloride solution
  7. dry with materialdried over sodium sulfate
  8. distillationdistilled under reduced pressure
  9. customto remove the solvent