反应详情

1.0 g (3.3 mmol) of 4-(3-benzyloxyimino-2-oxovaleryl)morpholine was dissolved in 20 ml of 2-propanol and 1.24 g (6.6 mmol) of 4-methoxybenzylhydrazine hydrochloride, 1.08 g (13.2 mmol) of sodium acetate and 1 ml of acetic acid were added and the mixture was refluxed for 15 hours. After distilling the solvent off under reduced pressure, 20 ml of water was added and the mixture was extracted three times with 30 ml of diethylether. After washing with 1N aqueous hydrochloric acid, water, a saturated aqueous sodium bicarbonate, water and then 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 1.19 g (yield: 83%) of 4-(3-benzyloxyimino-2-(4-methoxybenzylhydrazono)valeryl)morpholine as a yellow oil.

1. temperaturethe mixture was refluxed for 15 hours
2. distillationAfter distilling the solvent off under reduced pressure, 20 ml of water
3. additionwas added
4. extractionthe mixture was extracted three times with 30 ml of diethylether
5. washAfter washing with 1N aqueous hydrochloric acid, water
6. dry with materialby drying over with anhydrous magnesium sulfate
7. distillationthe solvent was distilled off under reduced pressure
8. customto obtain a residue, which
9. customwas purified by a column chromatography on a silica gel (n-hexane/ethyl acetate)