HRID1269880
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux for 1 hour
- customThe solid was removed by filtration
- distillationthe solvent was distilled off under reduced pressure
- additionEthyl acetate/water was added to the residue
- extractionfollowed by extraction with ethyl acetate
- washthe extract solution was washed with a saturated aqueous sodium chloride solution
- dry with materialdried over sodium sulfate
- distillationdistilled under reduced pressure
- customto remove the solvent