反应详情

温度

80 °C

A 50 mL round-bottomed flask was charged with N-(4-(1-(4-methoxybenzyl)-3-(4-(methylcarbamoyl)phenyl)-1H-pyrazolo[3,4-b]pyridin-4-yloxy)-3-fluorophenyl)-1-methyl-2-oxopyrrolidine-3-carboxamide (10.8 mg, 0.0173 mmol) and CF3COOH (2 mL). The reaction mixture was stirred at 80° C. for 4 hours. Then the CF3COOH was removed under reduced pressure. The residue was purified by silica gel chromatography (DCM/7 M NH3 in MeOH from 50/1 to 10/1, v/v) to afford product (3.9 mg, 44.7%). LRMS (APCI pos): >99% purity, 254 nm, m/e 503 (M+1). 1H NMR (400 MHz, CD3OD) δ 8.35 (d, 1H), 8.10 (d, 2H), 7.83-7.90 (m, 3H), 7.40 (d, 1H), 7.32 (t, 1H), 6.40 (d, 1H), 3.44-3.60 (m, 3H), 2.92 (s, 3H), 2.90 (s, 3H), 2.28-2.51 (m, 2H).

1. customThen the CF3COOH was removed under reduced pressure
2. customThe residue was purified by silica gel chromatography (DCM/7 M NH3 in MeOH from 50/1 to 10/1