反应详情

温度

50 °C

To a solution of 5-ethyl-2-fluoro-4-[3-(1,4,5,6,7,8-hexahydro-imidazo[4,5-d]azepin-2-yl)-1H-indazol-6-yl]-phenol trihydrobromide salt (Preparation 32, 50 mg, 80 μmol) in DMF (1 mL), was added benzyl bromide (14.4 mg, 10 μL, 85 μmol), and DIPEA (56 μL, 320 μmol). The reaction mixture was heated at 50° C. for 18 hours. The reaction mixture was then cooled to room temperature and partitioned between EtOAc (50 mL) and water (50 mL). The organic layer was washed with brine (50 mL), dried over sodium sulfate and concentrated in vacuo to furnish a brown oil. The crude material was purified by reverse phase chromatography (Method C) to afford 4 mg of the title compound.

1. temperatureThe reaction mixture was then cooled to room temperature
2. custompartitioned between EtOAc (50 mL) and water (50 mL)
3. washThe organic layer was washed with brine (50 mL)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customto furnish a brown oil
7. customThe crude material was purified by reverse phase chromatography (Method C)