反应详情

温度

80 °C

A mixture of tert-butyl 4-(5-bromopyrimidin-2-yl)piperazine-1-carboxylate (5.0 g, 14.6 mmol), palladium diacetate (240 mg, 1.46 mmol), triphenylphosphine (376 mg, 2.92 mmol) and tributyl(1-ethoxyvinyl)stannane (5.3 mL, 16.1 mL) in dioxane (100 mL) was degassed with nitrogen for three times, and the reaction mixture was stirred at 80° C. overnight. The reaction was cooled to RT and diluted with THF (100 mL), followed by the addition of 2 N HCl (100 mL). The mixture was stirred at RT for 30 mins, and LCMS showed the reaction was completed. The reaction mixture was diluted with ethyl acetate (200 mL). The organic phase was separated, washed with water (3×100 mL), dried over sodium sulfate, filtered and concentrated. The residue was purified by silica gel chromatography to afford the title compound (3.0 g, 67%). MS (ES+) C15H22N4O3 requires: 306. found: 251 [M−56+H]+.

1. customwas degassed with nitrogen for three times
2. temperatureThe reaction was cooled to RT
3. additiondiluted with THF (100 mL)
4. additionfollowed by the addition of 2 N HCl (100 mL)
5. stirringThe mixture was stirred at RT for 30 mins
6. additionThe reaction mixture was diluted with ethyl acetate (200 mL)
7. customThe organic phase was separated
8. washwashed with water (3×100 mL)
9. dry with materialdried over sodium sulfate
10. filtrationfiltered
11. concentrationconcentrated
12. customThe residue was purified by silica gel chromatography