反应详情

温度

40 °C

Aqueous sodium hydroxide (127 μL, 1 M, 0.127 mmol) was added to a solution of tert-butyl 4-(6-(4-fluorophenylamino)-1-(methylsulfonyl)-1H-pyrrolo[3,2-c]pyridin-2-yl)-1H-pyrazole-1-carboxylate (Preparation 53, 20 mg, 0.042 mmol) (mixed with some tert-butyl 4-(6-chloro-1-(methylsulfonyl)-1H-pyrrolo[3,2-c]pyridin-2-yl)-1H-pyrazole-1-carboxylate) in EtOH (339 μL). The reaction mixture was stirred for 4 hours at 40° C. The reaction mixture was filtered on SCX-2 column and was then purified using preparative TLC eluting with DCM/MeOH, 95/5 to afford the title compound as a white solid (7 mg, 20%). 1H NMR (500 MHz, CD3OD): δ 3.02 (s, 3H), 6.73 (d, J=0.8 Hz, 1H), 7.00-7.07 (m, 2H), 7.45-7.49 (m, 2H), 7.51 (t, J=0.8 Hz, 1H), 7.90 (br s, 2H), 8.40 (d, J=0.8 Hz, 1H). ESI-HRMS Found 372.0936, calculated for C17H15FN5O2S [M+H]+: 372.0925. MPS1 IC50 (uM): 6.43

1. filtrationThe reaction mixture was filtered on SCX-2 column
2. customwas then purified
3. washeluting with DCM/MeOH, 95/5