反应详情

Trifluoromethyl(3,4-methylenedioxyphenyl) methanone (1.46 g, 0.0067 mole), hydroxylamine hydrochloride (1.06 g), 0.015 mole) and sodium acetate (0.86 g, 0.010 mole) were dissolved in a mixture of methanol (4 ml) and water (4 ml) and heated to reflux for 4.5 hours. After cooling to room temperature, water (10 ml) was added and the mixture extracted with ether (3×15 ml). The combined extracts were washed with water (20 ml) and brine (20 ml) and dried over anhydrous sodium sulfate. After filtration and removal of the solvent in vacuo the residue was recrystallized from a mixture of dichloromethane and petroleum spirit (40°-60° C.) to give trifluoromethyl(3,4-methylenedioxyphenyl)methanone-oxime (1.2 g), (76.9%) m.p. 96.0° C.

1. temperatureheated
2. temperatureto reflux for 4.5 hours
3. extractionthe mixture extracted with ether (3×15 ml)
4. washThe combined extracts were washed with water (20 ml) and brine (20 ml)
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationAfter filtration and removal of the solvent in vacuo the residue
7. customwas recrystallized from a mixture of dichloromethane and petroleum spirit (40°-60° C.)