反应详情

温度

90 °C

Under argon atmosphere, 4-(5-bromopyrimidin-2-yl)morpholine (700 mg) and tert-butyl piperazine-1-carboxylate (800 mg) were mixed with toluene (10 ml), and Pd2(dba)3 (130 mg), BINAP (260 mg), and potassium tert-butoxide (500 mg) were added thereto, followed by stirring at 90° C. overnight. The reaction mixture was cooled to room temperature, the reaction mixture was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane/EtOAc). The purified product thus obtained was mixed with EtOH (10 ml), and 4 M hydrogen chloride/dioxane (7 ml) was added thereto, followed by stirring at room temperature overnight. The reaction mixture was concentrated under reduced pressure, and CHCl3 and a saturated aqueous sodium hydrogen carbonate solution were then added thereto. The organic layer was dried over Na2SO4 and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (CHCl3/MeOH) to obtain 4-[5-(piperazin-1-yl)pyrimidin-2-yl]morpholine (239 mg).

1. additionwere added
2. temperatureThe reaction mixture was cooled to room temperature
3. concentrationthe reaction mixture was concentrated under reduced pressure
4. customthe residue was purified by silica gel column chromatography (hexane/EtOAc)
5. customThe purified product thus obtained
6. additionwas added
7. stirringby stirring at room temperature overnight
8. concentrationThe reaction mixture was concentrated under reduced pressure, and CHCl3
9. additiona saturated aqueous sodium hydrogen carbonate solution were then added
10. dry with materialThe organic layer was dried over Na2SO4
11. concentrationconcentrated under reduced pressure
12. customThe obtained residue was purified by silica gel column chromatography (CHCl3/MeOH)