反应详情

To a solution of methyl 4-trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo[3.1.0]hexane-1-carboxylate (1.52 g, 0.005 mole) in 10 ml of hexamethylphosphoric triamide was added lithium chloride (0.42 g, 0.010 mole). After heating at 75° for two hours, the cooled reaction mixture was diluted with ether. The ethereal solution was washed with water, dried over magnesium sulfate, and the ether was removed by evaporation, yielding a residue which was purified by column chromatography on silica gel using 9/1 n-hexane/ethylacetate as the eluent to give 4-trichloromethyl-6,6-dimethyl-2-oxo-3-oxabicyclo[3.1.0]hexane (0.34 g, 28% yield) as an oil.

1. temperatureAfter heating at 75° for two hours
2. customthe cooled reaction mixture
3. washThe ethereal solution was washed with water
4. dry with materialdried over magnesium sulfate
5. customthe ether was removed by evaporation
6. customyielding a residue which
7. customwas purified by column chromatography on silica gel using 9/1 n-hexane/ethylacetate as the eluent