反应详情

温度

25 °C

A solution of B5 and trifluoroethanol (120 mL) was treated with triethylamine (TEA) (16.6 mL) and stirred at 25° C. for 1 hour. In a separate reaction flask, a solution of 2,4-dichloro-5-trifluoromethylpyrimidine (13.2 g, 60.8 mmol) and trifluoroethanol (120 mL) was cooled to −45° C. The cold 2,4-dichloro-5-trifluoromethylpyrimidine solution was then treated drop-wise with the solution containing B5 and stirred at −45° C. for 2 hours. The mixture was allowed to warm to 25° C., and it was stirred at 25° C. for about 20 hours. The reaction mixture was then concentrated and cooled to 0° C. The resultant white mixture was diluted with EtOAc (15 ml), and the solids collected by filtration. The white solids were then washed with water and EtOAc to provide C9. Yield: 0.7 g, 45%. 1H NMR (400 MHz, d6-DMSO) δ: 3.07 (s, 3H), 3.29(s, 3H), 4.68 (d, 2H), 7.39 (m, 1H), 7.72 (d, 1H), 8.40 (s, 1H), 8.50 (t, 1H); ESI-MS: 396.0 (MH+).

1. customIn a separate reaction flask
2. stirringstirred at −45° C. for 2 hours
3. temperatureto warm to 25° C.
4. stirringit was stirred at 25° C. for about 20 hours
5. concentrationThe reaction mixture was then concentrated
6. temperaturecooled to 0° C
7. additionThe resultant white mixture was diluted with EtOAc (15 ml)
8. filtrationthe solids collected by filtration
9. washThe white solids were then washed with water and EtOAc