反应详情

温度

70 °C

To a solution of 5-phenylfuro[2,3-d]pyrimidin-4(3H)-one (2 g, 9.42 mmol, prepared as described in WO2006/004658) in DMF (20 ml) was charged cesium carbonate (6.76 g, 20.7 mmol) and 1,1,1-trifluoro-2-iodoethane (1.86 ml, 18.9 mmol). The reaction was heated at 70° C. for 18 h under a nitrogen atmosphere. A further 1 eq. of 1,1,1-trifluoro-2-iodoethane was charged to the reaction mixture. The reaction was heated to 100° C. for 5 h before being cooled to RT, diluted with water and extracted twice with ethyl acetate. The organic extracts were washed with brine (3×50 ml), dried (Na2SO4), filtered and concentrated in vacuo. The resultant residue was purified by silica gel chromatography (SiO2, 0 to 50% EtOAc in cyclohexane) affording the title compound as a beige solid (730 mg, 26%). LCMS RT=1.27 min, M+H+=295.

1. temperatureThe reaction was heated to 100° C. for 5 h
2. temperaturebefore being cooled to RT
3. extractionextracted twice with ethyl acetate
4. washThe organic extracts were washed with brine (3×50 ml)
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe resultant residue was purified by silica gel chromatography (SiO2, 0 to 50% EtOAc in cyclohexane)