反应详情

温度

10 °C

A quantity (18.4 g.) of 4-chromanone was dissolved in 100 ml. ethanol with heating to the boiling temperature. To this hot solution was added 18.4 g. hydroxylamine hydrochloride and a hot aqueous solution of sodium acetate (36.8 g.) that had been dissolved in 50 ml. water heated on a steam bath. The reaction mixture was heated at the reflux temperature for 1.5 hrs. when a thin layer chromatogram indicated that the reaction was completed. After cooling the mixture to about 10° C., crystals formed. The crystals were collected on a filter, washed with water, and dried in air. There was thus obtained 18.63 g. of 4-chromanone oxime that had a melting point at 139° to 142° C. Recrystallization from methanol gave 16.5 g. of the compound having the same melting point (139° to 142° C.).

1. additionTo this hot solution was added 18.4 g
2. temperatureThe reaction mixture was heated at the reflux temperature for 1.5 hrs
3. customcrystals formed
4. customThe crystals were collected on a filter
5. washwashed with water
6. customdried in air
7. customat 139° to 142° C
8. customRecrystallization from methanol
9. customgave 16.5 g
10. customthe same melting point (139° to 142° C.)