反应详情

温度

130 °C

A mixture of 2,6-dichloro-N-[(1S)-1-(5-fluoropyridin-2-yl)ethyl]pyrimidin-4-amine (Preparation 10a, 0.66 g, 2.31 mmol), 4-(tert-butyl-dimethylsilanyloxy)piperidine (prepared as described in WO2004/006926, 0.60 g, 2.77 mmol) and cesium carbonate (1.13 g, 3.46 mmol) in N,N′-dimethylformamide (15 mL) was stirred and heated to 130° C. in a sealed tube for 2 hours. After cooling to ambient temperature, water was added and the resulting mixture was extracted with ethyl acetate (×3). The combined organic extract was washed with water and brine, dried (MgSO4), filtered and the solvent was evaporated under reduced pressure. The residue was purified by flash chromatography (hexanes to 6:4 hexanes/ethyl acetate) to give the title compound (0.53 g, 50%) as a white solid.

1. temperatureAfter cooling to ambient temperature
2. extractionthe resulting mixture was extracted with ethyl acetate (×3)
3. extractionThe combined organic extract
4. washwas washed with water and brine
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customthe solvent was evaporated under reduced pressure
8. customThe residue was purified by flash chromatography (hexanes to 6:4 hexanes/ethyl acetate)