反应详情

A solution of 3-[2-[(diethoxyphosphoryl)acetyl]hydrazino]-1-hydroxy-7-trifluoromethylquinoxalin-2(1H)-one (438 mg, 1 mmol) and triphenylphosphine (525 mg, 2 mmol) in 25 ml of glacial acetic acid was heated under reflux overnight (ca. 15 h). The mixture was evaporated to dryness, and the residue was flash chromatographed (SiO2) with dichloromethane to remove excess triphenylphosphine, then with ethyl acetate to remove triphenylphosphine oxide, and finally with 5% acetic acid in ethyl acetate to give 161 mg (40%) of the title compound. M.p. 224°-226° C., dec. (ethanol).

1. temperatureunder reflux overnight (ca. 15 h)
2. customThe mixture was evaporated to dryness
3. customchromatographed (SiO2) with dichloromethane
4. customto remove excess triphenylphosphine
5. customwith ethyl acetate to remove triphenylphosphine oxide