反应详情

5.5 Milliliters of thionyl chloride was added dropwise to a chloroform solution containing 16.1 g of 5,7-dimethyl-8-methoxy-9-hydroxy-1,2,3,4,4a,9a-hexahydrofluorene under ice-cooling. After completion of the addition, reaction was effected at the same temperature for 2 hours. The reaction mixture was washed successively with water twice, saturated aqueous sodium chloride solution and saturated sodium bicarbonate solution and dried with magnesium sulfate. Then, the solvent was distilled off and the residue was purified by a silica gel column chromatography (eluent: ethyl acetate:n-hexane=1:20) to obtain 13.26 g of 5,7-dimethyl-8-methoxy-2,3,4,4a-tetrahydro-1H-fluorene.

1. temperaturecooling
2. additionAfter completion of the addition, reaction
3. washThe reaction mixture was washed successively with water twice
4. dry with materialsaturated aqueous sodium chloride solution and saturated sodium bicarbonate solution and dried with magnesium sulfate
5. distillationThen, the solvent was distilled off
6. customthe residue was purified by a silica gel column chromatography (eluent: ethyl acetate:n-hexane=1:20)