反应详情

To a solution of 2-phenyl-1,3-dioxan-5-ol (484 mg) in anhydrous tetrahydrofuran (10 ml) at 0° C. was added 60% sodium hydride (110 mg) and the mixture was heated to reflux for 25 minutes. On allowing to cool to ambient temperature 4,6-Dichloro-2-[(2,3-difluorobenzyl)thio]pyrimidine (the product of step (ii) (75 mg) was added and the reaction was heated to reflux for a further 90 minutes. The reaction mixture was allowed to cool, diluted with water and extracted with ethyl acetate (×3). The combined organic layers were dried with magnesium sulfate, filtered and evaporated. The residue was purified by column chromatography on silica using a 95:5 to 90:10 mixture of iso-hexane and ethyl acetate as eluent to give the sub-title compound as a white solid. Yield: 350 mg

1. temperaturethe mixture was heated
2. temperatureto reflux for 25 minutes
3. additionwas added
4. temperaturethe reaction was heated
5. temperatureto reflux for a further 90 minutes
6. temperatureto cool
7. extractionextracted with ethyl acetate (×3)
8. dry with materialThe combined organic layers were dried with magnesium sulfate
9. filtrationfiltered
10. customevaporated
11. customThe residue was purified by column chromatography on silica using a 95:5
12. additionto 90:10 mixture of iso-hexane and ethyl acetate as eluent