反应详情

To a mixture of 2-(trifluoromethyl)quinazolin-4(3H)-one (12 g) and phosphorous oxychloride (100 ml) was added DMF (0.5 ml) and the mixture was refluxed under nitrogen for 16 h. The excess phosphorous oxychloride was distilled off and the residue was diluted with ethyl acetate (200 ml). The ethyl acetate layer was washed with 10% solution of sodium bicarbonate, water and brine. The solvent was dried and evaporated. The residue was purified by chromatography (silica gel: 60-120 mesh) eluting with pet ether/ethyl acetate (9/1) to afford 8 g (61%) of the titled compound as a pale yellow solid.

1. temperaturethe mixture was refluxed under nitrogen for 16 h
2. distillationThe excess phosphorous oxychloride was distilled off
3. additionthe residue was diluted with ethyl acetate (200 ml)
4. washThe ethyl acetate layer was washed with 10% solution of sodium bicarbonate, water and brine
5. customThe solvent was dried
6. customevaporated
7. customThe residue was purified by chromatography (silica gel: 60-120 mesh)
8. washeluting with pet ether/ethyl acetate (9/1)