反应详情

To a solution of 4,6-Dichloro-2-[(2,3-difluorobenzyl)thio]pyrimidine (the product of example 1 step ii) (2 g) in THF (20 mL) was added potassium tert-butoxide (0.8 g) and the reaction mixture was stirred at ambient temperature for 20 h. Further potassium tert-butoxide (0.8 g) was added and the reaction mixture was stirred at ambient temperature for 4 h. The mixture was diluted with H2O and extracted with EtOAc (×3). The combined organic layers were washed with H2O and dried (MgSO4), filtered and evaporated. The resulting oil was purified by column chromatography on silica gel using MeOH/DCM (99:1 to 98:2 gradient) as eluent to give the subtitle compound as a clear, colourless oil. Yield: 0.68 g

1. stirringthe reaction mixture was stirred at ambient temperature for 4 h
2. extractionextracted with EtOAc (×3)
3. washThe combined organic layers were washed with H2O
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customThe resulting oil was purified by column chromatography on silica gel