Diethyl Carbonate → HCID 89586101, Verbindung

Reaktionsgleichung

[C:1](=[O:8])([O:5][CH2:6][CH3:7])OCC.[H-].[Na+].[C:11]1([N:17]2[C:21]([C:22](=[O:24])[CH3:23])=[CH:20][CH:19]=[N:18]2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>O>[O:24]=[C:22]([C:21]1[N:17]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:18]=[CH:19][CH:20]=1)[CH2:23][C:1]([O:5][CH2:6][CH3:7])=[O:8]

Komponenten

Versuchsvorschrift

To a mixture of diethyl carbonate (20.0 mL) and 60% NaH (0.34 g) was added 1-(1-phenyl-1H-pyrazol-5-yl)ethanone (1.30 g) at room temperature, and the mixture was heated under reflux for 2 hr. To the reaction mixture was added water, and the mixture was extracted with dichloromethane. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate) to give the title compound (1.10 g).