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 solution containing 75 mg of [5-(3,5-dichlorophenylthio)-3-methyl-1H-pyrazol-4-yl]-phenyl-methanone in 2 ml of dry N,N-dimethylformamide (DMF) at rt under nitrogen was treated with 12 mg of sodium hydride. The mixture was then stirred for 2 min. To the mixture was added 25 μof 2-iodopropane. The mixture was then stirred for 20 min. To the mixture was added 2mnl of water and then the mixture was extracted with ethyl acetate three times. Combined extracts were washed with brine then dried over anhydrous magnesium sulphate, filtered and evaporated. The residue was purified by flash chromatography on silica gel using diethyl ether/hexane (1:7) for the elution to give 32 mg of [5-(3,5-dichlorophenylthio)-1-isopropyl-3-methyl-1H-pyrazol-4-yl]-phenyl-methanone as a colourless oil. Mass spectrum (ES) m/z 405[M+H]+.
WORKUP
后处理
- stirringThe mixture was then stirred for 20 min
- extractionthe mixture was extracted with ethyl acetate three times
- washCombined extracts were washed with brine
- dry with materialthen dried over anhydrous magnesium sulphate
- filtrationfiltered
- customevaporated
- customThe residue was purified by flash chromatography on silica gel
- washfor the elution