反应详情

Triethylamine (5.2 g) was added dropwise to a stirred solution of 5,5-dimethyl-4-phenyl cyclohexane-1,3-dione (10.8 g) and n-butyryl chloride (5.3 g) in methylene chloride (100 ml). After stirring at ambient temperature for a further 2 hours, the reaction solution was washed with water and brine and dried over anhydrous magnesium sulphate. The methylene chloride was removed in vacuo to give a mixture of 1-butyryloxy-5,5-di-methyl-4-phenyl cyclohex-1-ene-3-one and 1-butyryloxy-5,5-dimethyl-6-phenyl cyclohex-1-ene-3-one. Toluene (100 ml) was added, followed by 4-(N-dimethylamino) pyridine (1 g) and the mixture was refluxed for 3 hours. Evaporation of the toluene in vacuo gave a red oil which was purified on a silica gel column using 5% (v/v) diethyl ethermethylene chloride as eluant to give the title compound (6 g) as a pale yellow oil.

1. washthe reaction solution was washed with water and brine
2. dry with materialdried over anhydrous magnesium sulphate
3. customThe methylene chloride was removed in vacuo
4. customto give
5. temperaturethe mixture was refluxed for 3 hours
6. customEvaporation of the toluene in vacuo
7. customgave a red oil which
8. customwas purified on a silica gel column