反应详情

Zinc dust (1.57 g) was added in portions to a suspension of 1-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-phenyl-1,2-ethanedione 1-oxime (856 mg) in a mixture acetic anhydride (1.7 ml) and AcOH (10 ml) under ambient temperature and the mixture was stirred at the same temperature for 4 hours. An insoluble material was filtered off and a filtrate was concentrated under reduced pressure to give a residue. The residue was dissolved in EtOAc, washed with sat. aq. NaHCO3 solution, dried over MgSO4 and subjected to column chromatography on silica gel eluting with a mixture of MeOH and EtOAc (2:98 v/v) to give N-[1-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-oxo-2-phenylethyl]acetamide as a solid (724 mg).

1. filtrationAn insoluble material was filtered off
2. concentrationa filtrate was concentrated under reduced pressure
3. customto give a residue
4. washwashed with sat. aq. NaHCO3 solution
5. dry with materialdried over MgSO4
6. additionsubjected to column chromatography on silica gel eluting with a mixture of MeOH and EtOAc (2:98 v/v)