反应详情

3.42 Grams of 60% sodium hydride was gradually added to a solution prepared by dissolving 17.7 g of 5,7-dimethyl-8-methoxy-1,2,3,4,4a,9a-hexahydro-9-fluorenone in 100 ml of dimethylformamide under ice-cooling, followed by stirring at room temperature for 30 minutes. Then, 5.4 ml of methyl iodide was added thereto under ice-cooling, followed by stirring at room temperature for 1 hour. The reaction mixture was poured into 3 liters of water and extracted with chloroform. 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=1:20) to obtain 9.6 g of 5,7,9a-trimethyl-8-methoxy-1,2,3,4,4a,9a-hexahydro-9fluorenone. fluorenone.

1. customprepared
2. temperaturecooling
3. temperatureunder ice-cooling
4. stirringby stirring at room temperature for 1 hour
5. extractionextracted with chloroform
6. dry with materialThe organic layer was dried with magnesium sulfate
7. distillationthe solvent was distilled off
8. customThe residue was purified by a silica gel column chromatography (eluent: ethyl acetate:n-hexane=1:20)