反应详情

A mixture of 3.96 g (20 mmol) of the above benzimidazole, 4.70 g (20 mmol) of 2,4-dichloro-6-(4-morpholinyl)-1,3,5-triazine, and 22 g (80 mmol) of powdered K2CO3 in 150 mL of DMF at room temperature was stirred rapidly for 3 hr and then diluted with water. The resulting precipitate was collected, washed with water, and then with cold ethanol, and dried to give 6.82 g (86%) of 1-[4-chloro-6-(4-morpholinyl)-1,3,5-triazin-2-yl]-2-(difluoromethyl)-4-methoxy-1H-benzimidazole: mp (CHCl3/EtOH) 263-266° C.; 1H NMR (CDCl3) δ 7.99 (d, J=8.4 Hz, 1H), 7.48 (t, JHF=53.4 Hz, 1H), 7.40 (t, J=8.3 Hz, 1H), 6.86 (d, J=8.1 Hz, 1H), 4.05 (s, 3H), 3.96 (m, 4H), 3.82 (m, 4H); Anal. Calcd. for C16H15ClF2N6O2: C, 48.4; H, 3.8; N, 21.2. Found: C, 48.3; H, 3.8; N, 21.1%.

1. customThe resulting precipitate was collected
2. washwashed with water
3. dry with materialwith cold ethanol, and dried