反应详情

To a solution of 15.0 g (103 mmol) of methyl 2-hydroxyiminoacetoacetate in 200 ml of acetone, 14.4 g (113 mmol) of benzyl chloride and 21.4 g (155 mmol) of potassium carbonate were added and the mixture was heated under reflux for 15 hours. The reaction mixture was combined with 200 ml of water and extracted three times with 200 ml of diethylether. After washing with water and a saturated aqueous sodium chloride followed by drying over with anhydrous magnesium sulfate, 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 18.7 g (yield: 77%) of methyl 2-benzyloxyiminoacetoacetate as a colorless crystal.

1. temperaturethe mixture was heated
2. temperatureunder reflux for 15 hours
3. extractionextracted three times with 200 ml of diethylether
4. washAfter washing with water
5. dry with materialby drying 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)