反应详情

To 4,4-Dimethylcyclohexanone (50 g, 396.19 mmol), NH2OH.HCl (35.84 g, 515.75 mmol) in H2O (190 mL) and ethanol (250 mL) was added a solution of Na2CO3 (54.16 g, 510.99 mmol) in water (170 mL) dropwise over a period of 20 minutes. After complete addition, reaction mixture was heated to reflux for 3h. The ethanol was evaporated, and the residue extracted into ethyl acetate (4×120 mL). The combined organic layer was washed with water (150 mL), brine (150 mL) and dried over sodium sulfate and concentrated to afford 45 g (80.4%) 4,4-dimethyl cyclohexanone oxime (I 6a) as white solid.

1. additionAfter complete addition, reaction mixture
2. temperaturewas heated
3. temperatureto reflux for 3h
4. customThe ethanol was evaporated
5. extractionthe residue extracted into ethyl acetate (4×120 mL)
6. washThe combined organic layer was washed with water (150 mL), brine (150 mL)
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated