反应详情

A single-neck, round-bottomed flask was charged with tert-butyl 4-(7-(2-fluoro -4-(2-(4-fluorophenyl)-3-oxo-2,3-dihydropyridazine-4-carboxamido)phenoxy)thieno[3,2-b]pyridin-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate (27.3 mg, 0.0415 mmol) and CF3CO2H (5 mL). The reaction mixture was stirred at room temperature until the starting material had been consumed (four hours). Then the solvent was removed and 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 (16.7 mg, 72.2%). LRMS (APCI pos): >99% purity, 254 nm, m/e 558 (M+1). 1H NMR (400 MHz, CDCl3) δ 11.83 (s, 1H), 8.42 (m, 2H), 8.24 (d, 1H), 7.95 (dd, 1H), 7.60 (m, 2H), 7.38 (m, 2H), 7.24 (m, 3H), 6.48 (d, 1H), 6.40 (s, 1H), 3.59 (m, 2H), 3.15 (m, 2H), 2.58 (m, 2H).

1. customhad been consumed (four hours)
2. customThen the solvent was removed
3. customthe residue was purified by silica gel chromatography (DCM/7 M NH3 in MeOH from 50/1 to 10/1