反应详情

Desoxyanisoin (98%, 52.2 g., 0.2 mole) and hydroxylamine hydrochloride (15.3 g., 0.22 mole) are slurried in a mixture of methanol (300 ml) and water (200 ml) and sodium hydroxide (16 g., 0.4 mole) is added slowly. The mixture is stirred for 15 minutes, then placed in a hot water bath (70° C.) and stirred an additional hour. Methanol is then added to the hot mixture until solution is almost complete, the mixture is filtered and concentrated to remove most of the methanol, then cooled with the addition of ice-water. Filtered, dissolved the resulting solid in ethyl acetate, extracted with brine. Dried the organic layer (Na2SO4), filtered and concentrated to obtain 53.5 g (98.5%) of the oxime as a yellow solid.

1. additionis added slowly
2. customplaced in a hot water bath
3. stirring(70° C.) and stirred an additional hour
4. filtrationthe mixture is filtered
5. concentrationconcentrated
6. customto remove most of the methanol
7. temperaturecooled with the addition of ice-water
8. filtrationFiltered
9. dissolutiondissolved the resulting solid in ethyl acetate
10. extractionextracted with brine
11. dry with materialDried the organic layer (Na2SO4)
12. filtrationfiltered
13. concentrationconcentrated