HRID79259
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
CONDITIONS
反应条件
- 温度
- 85 °C
PROCEDURE
实验过程
A mixture of 1-benzyl-3-ethyl-4-nitro-1H-indazole (46.0 mg, 0.164 mmol), iron powder (91.3 mg, 1.64 mmol) and ammonium chloride (4.4 mg, 0.082 mmol) was stirred in a 4:1 mixture of ethanol and water (5 mL) with heating to 85° C. for 60 minutes. The solvent was removed under reduced pressure. Ethyl acetate (4 mL) and triethylamine (1 mL) was added and the mixture was heated for 15 minutes at 85° C. After cooling, the mixture was filtered through glass fiber filter paper, rinsing with methanol, dichloromethane and ethyl acetate. The filtrate was concentrated under reduced pressure to provide 1-benzyl-3-ethyl-1H-indazol-4-amine as an oil (40 mg).
WORKUP
后处理
- customThe solvent was removed under reduced pressure
- additionEthyl acetate (4 mL) and triethylamine (1 mL) was added
- temperaturethe mixture was heated for 15 minutes at 85° C
- temperatureAfter cooling
- filtrationthe mixture was filtered through glass fiber
- filtrationfilter paper
- washrinsing with methanol, dichloromethane and ethyl acetate
- concentrationThe filtrate was concentrated under reduced pressure