反应详情

温度

100 °C

6-chloro-3-(4-fluorophenyl)-1-trityl-1H-pyrazolo[4,3-c]pyridine (Intermediate 4a, 73 mg, 0.147 mmol), (R)-1-(1-phenylethyl)urea (37 mg, 0.225 mmol), Cs2CO3 (120 mg, 0.367 mmol), BrettPhos precatalyst (11.7 mg, 0.015 mmol) and DMA (1.1 mL) were charged in a vial. The mixture was evacuated and purged with nitrogen six times and heated at 100° C. for 55 min. The mixture was diluted with EtOAc and washed with water, brine, dried (Na2SO4) and concentrated to afford a residue, which was purified by chromatography on silica gel (0-100% ethyl acetate in hexane, 20 CV) to afford (R)-1-(3-(4-fluorophenyl)-1-trityl-1H-pyrazolo[4,3-c]pyridin-6-yl)-3-(1-phenylethyl)urea (85 mg, 0.136 mmol, 92%) as a yellow solid. MS ESI calcd. For C40H32FN5O [M+H]+ 618, found 618.

1. customThe mixture was evacuated
2. custompurged with nitrogen six times
3. additionThe mixture was diluted with EtOAc
4. washwashed with water, brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customto afford a residue, which
8. customwas purified by chromatography on silica gel (0-100% ethyl acetate in hexane, 20 CV)