反应详情

7.99 Grams of hydroxylamine hydrochloride was added to a solution prepared by dissolving 17.22 g of 5,7-dimethyl-8-hydroxy-1,2,3,4,4a,9a-hexahydro-9-fluorenone in 100 ml of pyridine and the mixture was refluxed under heating for 2 hours. Pyridine was distilled off under reduced pressure and the resulting residue was extracted with 300 ml of chloroform. The extract was washed with water 1% hydrochloric acid and then with saturated aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate. After the solvent was distilled off, the product was recrystallized from ethanol to obtain 11.56 g of 5,7-dimethyl-8-hydroxy-1,2,3,4,4a,9a-hexahydro-9-fluorenone oxime as a mixture of syn-isomer and anti-isomer.

1. customprepared
2. temperaturethe mixture was refluxed
3. temperatureunder heating for 2 hours
4. distillationPyridine was distilled off under reduced pressure
5. extractionthe resulting residue was extracted with 300 ml of chloroform
6. washThe extract was washed with water 1% hydrochloric acid
7. dry with materialwith saturated aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate
8. distillationAfter the solvent was distilled off
9. customthe product was recrystallized from ethanol