HRID47615

反应详情

EQUATION

反应方程式

HRID 47615 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 μl of 2-iodopropane. The mixture was then stirred for 20 min. To the mixture was added 2 ml 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 7; 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

  1. stirringThe mixture was then stirred for 20 min
  2. extractionthe mixture was extracted with ethyl acetate three times
  3. washCombined extracts were washed with brine
  4. dry with materialthen dried over anhydrous magnesium sulphate
  5. filtrationfiltered
  6. customevaporated
  7. customwas purified by flash chromatography on silica gel
  8. washfor the elution