反应详情

To a solution of 2,4-difluoro-6-({2-{[4-[4-(1-methylethyl)-1-piperazinyl]-2-(methyloxy)phenyl]amino}-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)benzamide (1.5 g, 2.17 mmols) in 1,4-dioxane (100 ml) and 2-propanol (2 ml) was added 1.0M potassium hydroxide (21 ml, 21.7 mmol) and the reaction was heated at 80C overnight. The resulting solution was diluted with ethyl acetate, washed with water, adsorbed onto silica gel and purified by LC (DCM to 10% MeOH/DCM) to afford 2,4-difluoro-6-[(2-{[4-[4-(1-methylethyl)-1-piperazinyl]-2-(methyloxy)phenyl]amino}-1H-pyrrolo[2,3-d]pyrimidin-4-yl)amino]benzamide (1.0 g, 86%). ESIMS (M+H)+=537. 1H NMR (400 MHz, DMSO-d6) δ ppm 1.00 (d, J=6.60 Hz, 6H) 2.54-2.60 (m, 4H) 2.64-2.72 (m, 1H) 3.05-3.11(m, 4H) 3.78 (s, 3H) 6.18 (dd, J=3.48, 2.02 Hz, 1H) 6.45 (dd, J=8.62, 2.38 Hz, 1H) 6.61 (d, J=2.57 Hz, 1H) 6.86-6.92 (m, 1H) 6.96 (dd, J=3.67, 2.20 Hz, 1H) 7.59 (s, 1H) 7.68 (d, J=8.80 Hz, 1H) 8.01 (br. s., 1H) 8.16 (s, 1H) 8.53-8.59 (m, 1H) 11.08 (s, 1H) 11.32 (s, 1H).

1. washwashed with water
2. custompurified by LC (DCM to 10% MeOH/DCM)