反应详情

温度

70 °C

To a mixture of 3-chloro-2-(4-(2,4-difluorophenoxyl)piperidin-1-yl)pyrido[3,4-b]pyrazine (2.5 g, 6.64 mmol) in DMF (30 mL) was added (S)-tetrahydrofuran-3-amine hydrochloride (4.10 g, 33.2 mmol) and Et3N (9.25 mL, 66.4 mmol) at room temperature. The reaction mixture was stirred at 70° C. for 14 h then cooled to room temperature and diluted with EtOAc (80 mL), washed with water (30 mL) and brine (2×30 mL). The organic layer was dried over Na2SO4 and concentrated in vacuo, then the residue was purified by column chromatography (petroleum ether:EtOAc from 10:1 to 1:1) on silica gel to give the title compound as a yellow solid (2.0 g). ESI-MS m/z [M+H]+ 428.1.

1. temperaturethen cooled to room temperature
2. washwashed with water (30 mL) and brine (2×30 mL)
3. dry with materialThe organic layer was dried over Na2SO4
4. concentrationconcentrated in vacuo
5. customthe residue was purified by column chromatography (petroleum ether:EtOAc from 10:1 to 1:1) on silica gel