HRID1640981
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
N-(5-benzenesulfonyl-1H-indazol-3-yl)-4-(4-methyl-piperazin-1-yl)-2-nitro-benzamide (1.71 g, 3.29 mmol) was suspended in a mixture of tetrahydrofuran (17 mL), ethanol (33 mL), water (25 mL) and cyclohexene (17 mL), treated with 10% palladium on carbon and stirred under reflux. After two hours the reaction was cooled to room temperature and filtered over celite washing thoroughly with tetrahydrofuran. Evaporation of the filtrate and purification of the crude product by flash chromatography over silica gel (eluent: dichloromethane/methanol/33% NH4OH in 95:5:1 ratio) afforded 1.39 g of title compound as a yellow powder (86% yield).
WORKUP
后处理
- temperatureunder reflux
- filtrationfiltered
- washover celite washing thoroughly with tetrahydrofuran
- customEvaporation of the filtrate and purification of the crude product by flash chromatography over silica gel (eluent: dichloromethane/methanol/33% NH4OH in 95:5:1 ratio)