反应详情

A solution of 3-(4-(chloromethyl)phenyl)-9H-benzo[f]pyrido[2,3-b][1,2,4]triazolo[4,3-d][1,4]diazepine (1.3 g, 3.62 mmol), tert-butyl piperidin-4-ylcarbamate (0.71 g, 3.80 mmol), triethylamine (1 mL) in dimethylacetamide (15 mL) was stirred at 75° C. for 20 hours. The mixture wass diluted with water (30 mL). The resulting suspension was stirred at room temperature. The solid was collected by filtration, washed thoroughly with water and dried under high vacuum. The tert-butyl (1-(4-(9H-benzo[f]pyrido[2,3-b][1,2,4]triazolo[4,3-d][1,4]diazepin-3-yl)benzyl)piperidin-4-yl)carbamate was obtained as a yellow solid (1.3 g, 69%). M.p.=145-147° C.; 400 MHz 1H NMR (DMSO-d6) δ: 8.76 (s, 1H), 8.18 (dd, J=4.4, 1.2 Hz, 1H), 7.93 (dd, J=8.0, 1.2 Hz, 1H), 7.41 (td, J=8.0, 1.6 Hz, 1H), 7.35-7.30 (m, 5H), 7.15-7.08 (m, 2H), 6.87 (dd, J=8.0, 4.8 Hz, 1H), 6.76 (d, J=8.4 Hz, 1H), 3.45 (s, 2H), 3.21-3.06 (m, 1H), 2.80-2.65 (m, 2H), 2.0-1.9 (m, 2H), 1.7-1.6 (m, 2H), 1.4-1.3 (m, 2H), 1.34 (s, 9H); LCMS [M+H]: 524.

1. filtrationThe solid was collected by filtration
2. washwashed thoroughly with water
3. customdried under high vacuum