反应详情

To a solution of 600 mg (3.2 mmol) of 3-hydroxyimino-2-methoxyimino-N,N-dimethylbutyramide in 20 ml of acetone, 500 mg (3.5 mmol) of 4-methylbenzylchloride and 660 mg (4.8 mmol) of potassium carbonate were added and the mixture was heated under reflux for 16 hours. The reaction mixture was combined with 30 ml of water and extracted three times with 30 ml of diethylether. After washing with water and a saturated aqueous sodium chloride, the mixture was dried over with anhydrous magnesium sulfate and then the solvent was distilled off. The residue thus obtained was purified by a column chromatography on a silica gel (n-hexane/ethyl acetate) to obtain 900 mg (yield: 96%) of 3-(4-methylbenzyloxyimino)-2-methoxyimino-N,N-dimethylbutyramide as a colorless crystal.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 16 hours
3. extractionextracted three times with 30 ml of diethylether
4. washAfter washing with water
5. dry with materiala saturated aqueous sodium chloride, the mixture was dried over with anhydrous magnesium sulfate
6. distillationthe solvent was distilled off
7. customThe residue thus obtained
8. customwas purified by a column chromatography on a silica gel (n-hexane/ethyl acetate)