反应详情

温度

90 °C

A mixture of 25 g of 5-methyl-8-hydroxy-1,2,3,4,4a,9a-hexahydro-9-fluorenone, 62.5 ml of acetic anhydride and 18.88 ml of bisdimethylaminomethane was stirred with heating at 90° C. for 2 hours. The reaction mixture was left to stand for cooling and then to the reaction mixture was added saturated aqueous sodium chloride solution, followed by extraction with dichloromethane. The organic layer was dried with magnesium sulfate and then the solvent was distilled off. The residue was purified by a silica gel column chromatography (eluent: ethyl acetate:n-hexane=1:10) to obtain 14.37 g of 7-dimethylaminomethyl-8-hydroxy-5-methyl-1,2,3,4,4a,9a-hexahydro-9-fluorenone.

1. waitThe reaction mixture was left
2. temperaturefor cooling
3. extractionfollowed by extraction with dichloromethane
4. dry with materialThe organic layer was dried with magnesium sulfate
5. distillationthe solvent was distilled off
6. customThe residue was purified by a silica gel column chromatography (eluent: ethyl acetate:n-hexane=1:10)