反应详情

温度

50 °C

A 20 mL sealable tube was charged with 4-(7-(4-amino-2-fluorophenoxy)thieno[3,2-b]pyridin-2-yl)-N-methylbenzamide (Example 95, Step A, 0.240 g, 0.610 mmol), 1-((4-fluorophenyl)carbamoyl)cyclopropanecarbonyl fluoride (0.172 g, 0.763 mmol), and acetonitrile (5 mL). The mixture was heated under nitrogen to 50° C. for 12 hours. The reaction was then cooled to room temperature and concentrated to dryness. The crude residue was purified by 3 triturations with hot acetonitrile to obtain product (202 mg, 64%) and as a white solid. LRMS (esi+) 599 m/z (M+1) detected. 1H NMR (d6-DMSO, 400 MHz) δ 10.41 (s, 1H), 10 (s, 1H), 8.55 (m, 2H), 8.20 (s, 1H), 8.00 (m, 5H), 7.64 (m, 2H), 7.52 (m, 2H), 7.16 (m, 2H), 6.65 (m, 1H), 2.82 (d, J=4 Hz, 3H), 1.48 (br s, 4H).

1. temperatureThe reaction was then cooled to room temperature
2. concentrationconcentrated to dryness
3. customThe crude residue was purified by 3 triturations with hot acetonitrile