HRID52333
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
A mixture of 2-(4-methylphenyl)-4-hydroxy-1-[4-(methylsulfonyl)phenyl]-4-trifluoromethyl-4,5-dihydro-1H-imidazole (10 mmol) and p-toluenesulfonic acid monohydrate (1 mmol) in toluene (100 mL) is heated to reflux for 72 hours. The reaction mixture is cooled and the solvent removed under reduced pressure. The crude residue is redissolved in methylene chloride and washed with water, aqueous sodium bicarbonate and brine. After drying (Na2SO4), filtration and concentration in vacuo, the crude mixture is chromatographed on silica gel using toluene/ethyl acetate to give pure 2-(4-methylphenyl)-1-[4-(methylsulfonyl)phenyl]-4-trifluoromethyl-1H-imidazole.
WORKUP
后处理
- temperatureis heated
- temperatureto reflux for 72 hours
- temperatureThe reaction mixture is cooled
- customthe solvent removed under reduced pressure
- dissolutionThe crude residue is redissolved in methylene chloride
- washwashed with water, aqueous sodium bicarbonate and brine
- customAfter drying
- filtration(Na2SO4), filtration and concentration in vacuo
- customthe crude mixture is chromatographed on silica gel