反应详情

温度

100 °C

DBU (2 μL, 0.016 mmol) was added to a solution of N-(4-fluorophenyl)-1-(methylsulfonyl)-2-(1H-pyrazol-4-yl)-1H-pyrrolo[3,2-c]pyridin-6-amine (Example 187, 3 mg, 8.08 μmol) in DMF (54 μL). The reaction mixture was stirred for 1 hour at 50° C. and for 1 hour at 100° C. The reaction mixture was diluted with water and the aqueous layer was extracted with EtOAc. The combined organic layers were dried over MgSO4, filtered and concentrated under reduced pressure. The residue was then purified using preparative TLC eluting with DCM/MeOH, 90/10 to afford the title compound as a brown solid (2 mg, 84%). 1H NMR (500 MHz, CD3OD): δ 6.60 (d, J=0.9 Hz), 6.85 (s, 1H), 6.99-7.06 (m, 2H), 7.26-7.32 (m, 2H), 8.00 (br s, 2H), 8.34 (s, 1H). ESI-HRMS Found 294.1158, calculated for C16H13FN5 [M+H]+: 294.1150. MPS1 IC50 (uM): 0.140

1. extractionthe aqueous layer was extracted with EtOAc
2. dry with materialThe combined organic layers were dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was then purified
6. washeluting with DCM/MeOH, 90/10