反应详情

27.5 g (67 mmol) of 1-(2-hydroxy-3-methylphenyl)-2-(triphenylphosphoranylidene)ethanone are heated to reflux in 200 ml of absolute toluene. 13.7 g (134 mmol) of acetic anhydride and 11.1 g (141 mmol) of pyridine are slowly added dropwise to this solution. The reaction mixture is then heated under reflux for 6 h. After cooling to room temperature, the solution is washed with saturated sodium carbonate solution and dried over sodium sulfate. The solvent is removed in vacuo, and the residue is purified by column chromatography (mobile phase: cyclohexane/ethyl acetate 7:3→4:6). 7.5 g (64% of theory) of the title compound are obtained.

1. temperatureThe reaction mixture is then heated
2. temperatureunder reflux for 6 h
3. washthe solution is washed with saturated sodium carbonate solution
4. dry with materialdried over sodium sulfate
5. customThe solvent is removed in vacuo
6. customthe residue is purified by column chromatography (mobile phase: cyclohexane/ethyl acetate 7:3→4:6)