反应详情

Under nitrogen atmosphere, 2-isopropyl-6-(2-oxo-5-phenyl-2,3-dihydro-oxazol-4-yl)-3(2H)-pyridazinone (100 mg) was added to a suspension of NaH (60% dispersion in mineral oil) (14 mg) in DMF (0.3 ml) at 20-25° C. and the mixture was stirred at the same temperature for 30 minutes. Methyl bromoacetate (0.0035 ml) was added to the mixture and stirred at 70-75° C. for 7 hours. After an addition of water (5 ml), an aqueous solution was removed by decantation to give a residue. The residue was dissolved in CHCl3, dried over MgSO4, concentrated under reduced pressure and subjected to column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (40:60 v/v) to give methyl [4-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-oxo-5-phenyl-oxazol-3(2H)-yl]-acetate as a solid (64 mg).

1. stirringstirred at 70-75° C. for 7 hours
2. customan aqueous solution was removed by decantation
3. customto give a residue
4. dry with materialdried over MgSO4
5. concentrationconcentrated under reduced pressure
6. additionsubjected to column chromatography on silica gel eluting with a mixture of n-hexane and EtOAc (40:60 v/v)