反应详情

温度

120 °C

To a suspension of 2-({2-{[1-(N,N-dimethylglycyl)-5-(methyloxy)-2,3-dihydro-1H-indol-6-yl]amino}-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-4,6-difluoro-N-methylbenzamide (0.950 g, 1.07 mmol) in 1,4 dioxane (10 mL) in a microwave vessel was added 6 N NaOH (10 ml) and water (3 mL). The resulting mixture was stirred in the microwave at 120° C. for 9 min. The reaction mixture was diluted with EtOAc and THF and the organic layer was washed with water and a saturated brine solution. Combined organic layers were dried over sodium sulfate and all solvents were removed under reduced pressure and purified via chromatography on SiO2 to afford 2-[(2-{[1-(N,N-dimethylglycyl)-5-(methyloxy)-2,3-dihydro-1H-indol-6-yl]amino}-1H-pyrrolo[2,3-d]pyrimidin-4-yl)amino]-4,6-difluoro-N-methylbenzamide (0.532 g, 0.966 mmol) as a beige solid. (ESIMS (M+H)+=551). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.23 (s, 6 H) 2.83 (d, J=4.40 Hz, 3 H) 3.06-3.12 (m, 2 H) 3.33 (s, 2 H) 3.76 (s, 2 H) 4.05-4.23 (m, 2 H) 6.25 (dd, J=3.39, 1.74 Hz, 1 H) 6.80-6.94 (m, 1 H) 6.93-7.04 (m, 2 H) 7.80 (s, 1 H) 8.41-8.54 (m, 2 H) 8.54-8.64 (m, 1 H) 10.79 (s, 1 H) 11.33 (br. s., 1 H)

1. washthe organic layer was washed with water
2. dry with materialCombined organic layers were dried over sodium sulfate
3. customall solvents were removed under reduced pressure
4. custompurified via chromatography on SiO2