反应详情

温度

120 °C

To a solution of 47.06 g (0.2 mol) of methyl 3-benzyloxyiminovalerate in 150 ml of chlorbenzene, 24.41 g (0.22 mol) of selenium dioxide was added and the mixture was stirred for 8 hours at 120° C. After adding 200 ml of water and filtering through Celite, the filtrate was 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 under reduced pressure to obtain a residue, which was purified by a column chromatography on a silica gel (n-hexane/ethyl acetate) to obtain 31.15 g (yield 62%) of methyl 3-benzyloxyimino-2-oxovalerate as a colorless oil.

1. filtrationfiltering through Celite
2. extractionthe filtrate was extracted three times with 200 ml of diethylether
3. washAfter washing with water
4. dry with materialby drying over with anhydrous magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customto obtain a residue, which
7. customwas purified by a column chromatography on a silica gel (n-hexane/ethyl acetate)