反应详情

500 Milligrams of hydroxylamine hydrochloride was added to an ethanol-chloroform (5:1) solution containing 910 mg of 5,7-dimethyl-8-methoxy-9-formylmethyl-1,2,3,4-tetrahydro-9H-fluorene in 18 ml of ethanol-chloroform and the mixture was refluxed with heating for 2 hours. The reaction mixture was diluted with chloroform and then washed with saturated aqueous sodium chloride solution and subsequently the solvent was distilled off. The residue was purified by a silica gel column chromatography (eluent: ethyl acetate:n-hexane=1:10) to obtain 670 mg of 5,7-dimethyl-8-methoxy-9-hydroxyiminomethyl-1,2,3,4-tetrahydro-9H-fluorene

1. temperaturethe mixture was refluxed
2. temperaturewith heating for 2 hours
3. washwashed with saturated aqueous sodium chloride solution
4. distillationsubsequently the solvent was distilled off
5. customThe residue was purified by a silica gel column chromatography (eluent: ethyl acetate:n-hexane=1:10)