反应详情

温度

180 °C

The title compound was synthesized by combining N-{3-[3-(2-chloro-4-pyrimidinyl)pyrazolo[1,5-a]pyridin-2-yl]phenyl}-2,6-difluorobenzamide (152 mg, 0.33 mmol), (5-amino-2,3-dihydro-1H-inden-2-yl)dimethylamine (70 mg, 0.40 mmol), hydrochloric acid (0.033 mmol, 33 uL 1M HCl/diethylether) and 3 mL isopropanol in a sealed vessel. The vial and contents were heated at 180° C. for 30 mins. The reaction was cooled and concentrated. The residue was partitioned between EtOAc and saturated aqueous NaHCO3. The organic layer was washed with brine, dried with MgSO4 and concentrated. The crude material was purified by silica gel column chromatography (0-100% gradient; (90% CH2Cl2:9% MeOH:1% NH4OH/CH2Cl2)) Purification provided 28 mg (14%) of the coupled adduct. ESIMS (M+H)+=603.30.

1. temperatureThe reaction was cooled
2. concentrationconcentrated
3. customThe residue was partitioned between EtOAc and saturated aqueous NaHCO3
4. washThe organic layer was washed with brine
5. dry with materialdried with MgSO4
6. concentrationconcentrated
7. customThe crude material was purified by silica gel column chromatography (0-100% gradient; (90% CH2Cl2:9% MeOH:1% NH4OH/CH2Cl2)) Purification