反应详情

6-Bromo-4H-pyrido[3,2-b][1,4]oxazin-3-one (10.0 g, 44 mmole) and trans-2-phenylvinylboronic acid (9.0 g, 61 mmole), were dissolved in 1,4-dioxane (200 mL) and the solution was degassed with argon. (Ph3P)4Pd (2.5 g, 2.2 mmole) was added, followed by a solution of K2CO3 (15 g, 109 mmole) in H2O (100 mL). The reaction was heated at reflux under argon overnight, then was cooled to room temperature and diluted with chloroform (400 mL). The solution was washed sequentially with H2O and brine, dried (Na2SO4), and concentrated in vacuo. The solid residue was recrystallized from hot EtOAc to afford the title compound (6.4 g, 57.5%): LC-MS (ES) m/e 253 (M+H)+.

1. customthe solution was degassed with argon
2. temperatureThe reaction was heated
3. temperatureat reflux under argon overnight
4. washThe solution was washed sequentially with H2O and brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customThe solid residue was recrystallized from hot EtOAc