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 2.56 g of 5-bromo-3-(3-fluorophenyl)-7-methyl-1H-indazole in 30 ml of dimethylformamide was added 0.50 g of sodium hydride at room temperature, and the mixture was stirred at the same temperature for 15 minutes. At the same temperature, 2.34 g of triphenylmethane chloride was added and the mixture was stirred at the same temperature for one day. Water was added to the reaction mixture and the mixture was diluted with ethyl acetate. The organic layer was sequentially washed with saturated aqueous ammonium chloride solution and brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:10) and the resulting crystals were washed with diethyl ether, to give 1.94 g of the title compound as colorless crystals.
WORKUP
后处理
- stirringthe mixture was stirred at the same temperature for one day
- washThe organic layer was sequentially washed with saturated aqueous ammonium chloride solution and brine
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was evaporated
- customThe crude product was purified
- customseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:10)
- washthe resulting crystals were washed with diethyl ether