反应详情

To a solution of 6-(difluoromethoxy)-2-[[(2,3-difluorophenyl)methyl]thio]-4-pyrimidinol (product of step i) (0.4 g) in 1,2-dimethoxyethane was added benzyltriethylammonium chloride (3 mg) and phosphorous oxychloride (0.23 mL). The resulting mixture was heated to reflux for 16 hours. The reaction mixture was cooled then diluted with H2O and extracted with EtOAc. The organic layer was washed with H2O and dried (MgSO4), filtered and evaporated. Purification was by column chromatography on silica gel using EtOAc/isohexane (2:8) as eluent to give the subtitle compound as a clear, colourless oil. Yield: 0.35 g

1. temperatureThe resulting mixture was heated
2. temperatureto reflux for 16 hours
3. temperatureThe reaction mixture was cooled
4. extractionextracted with EtOAc
5. washThe organic layer was washed with H2O
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customevaporated
9. customPurification