HRID1438414

反应详情

EQUATION

反应方程式

HRID 1438414 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred suspension of methyltriphenylphosphonium bromide (3.53 g, 9.89 mmol) in THF (30 ml) was added potassium tert-butoxide (1.11 g, 9.89 mmol) in THF (10 ml) dropwise at 0° C. and the mixture was stirred at ambient temperature for 2 hours. Then, to this mixture was added 4-(trifluoromethyl)propiophenone (Aldrich, 1.00 g, 4.95 mmol) in THF (10 ml) at 0° C. and stirred at ambient temperature for 2 hours. The reaction was quenched with small amount of water and evaporated to remove the solvent. The crude mixture was diluted with hexane. The formed precipitates were filtered and the organic layer was separated. After evaporation of solvent, residue was applied to a silica gel chromatography column and eluted with hexane to afford 1.12 g (crude 100%) of the title compound as a red oil.

WORKUP

后处理

  1. stirringstirred at ambient temperature for 2 hours
  2. customThe reaction was quenched with small amount of water
  3. customevaporated
  4. customto remove the solvent
  5. additionThe crude mixture was diluted with hexane
  6. customThe formed precipitates
  7. filtrationwere filtered
  8. customthe organic layer was separated
  9. customAfter evaporation of solvent, residue
  10. washeluted with hexane