反应详情

温度

80 °C

To a room temperature solution under nitrogen containing 0.20 g of N-[1-(4-bromo-3-fluorophenyl)-2-(4-morpholinyl)ethyl]-2-(6,7-dichloro-3-oxo-2,3-dihydro-4H-1,4-benzoxazin-4-yl)-N-methylacetamide (0.348 mmols) in 3.5 mL of dry DMF was added 0.09 g of {4-[(methylsulfonyl)amino]phenyl}boronic acid (0.418 mmols), 0.014 g of (dppf)PdCl2 (0.017 mmols), and 0.70 mL of Na2CO3 solution (2M in water). The reaction mixture was heated to 80° C. After 18 h the reaction was cooled to ambient temperature and filtered through a 0.2 □m syringe filter. The resulting DMF solution was purified by preparative HPLC (Phenomenex 50×100 mm column, 90 mL/min flow rate, A: 0.1% TFA in acetonitrile B: 0.1% TFA in water, A: 10 to 100% over 15 min, UV detection at 215 nm) to give 0.022 g (9%) of the title compound as a light brown solid. MS (ES) m/e 666, 667 [M+H]+.

1. temperatureAfter 18 h the reaction was cooled to ambient temperature
2. filtrationfiltered through a 0.2 □m syringe
3. filtrationfilter
4. customThe resulting DMF solution was purified by preparative HPLC (Phenomenex 50×100 mm column, 90 mL/min flow rate