反应详情

28 Grams of hydroxylamine hydrochloride and 56 g of potassium carbonate were added in 400 ml of methanol, and the mixture was refluxed by hetting for 30 minutes. After cooling the reaction mixture to a room temperature, the supernatant liquor was collected by separation to prepare a methanol solution of hydroxylamine. To this methanol solution of hydroxylamine was added 16.2 g of 7-hydroxy-4-methyl-1-indanone and refluxed by heating for 5 hours under stirring condition. The reaction mixture was concentrated to dryness under a reduced pressure. To the residue thus obtained was added 200 ml of ethyl acetate, then the insoluble matter was removed by filtration. The filtrate was concentrated to dryness under a reduced pressure, and the residue was recrystallized from methanol to obtain 17.6 g of 7-hydroxy-4-methyl-1-indanone oxime in the form of colorless needle-like crystals.

1. temperaturethe mixture was refluxed
2. customthe supernatant liquor was collected by separation
3. customto prepare a methanol solution of hydroxylamine
4. temperaturerefluxed
5. temperatureby heating for 5 hours
6. concentrationThe reaction mixture was concentrated to dryness under a reduced pressure
7. customTo the residue thus obtained
8. customthe insoluble matter was removed by filtration
9. concentrationThe filtrate was concentrated to dryness under a reduced pressure
10. customthe residue was recrystallized from methanol