反应详情

温度

80 °C

Under an argon atmosphere, 2.82 g (10 mmol) of [3-(5-bromopyrimidin-2-yl)-phenyl]methanol are dissolved in 100 ml of ethylene glycol dimethyl ether, 3.38 g (10 mmol) of 4-{2-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrazol-1-yl]ethyl}morpholine and 4.25 g (20 mmol) of tripotassium phosphate trihydrate are added. The reaction mixture is evacuated twice and flushed with argon. 840 mg (1.2 mmol) of bis(triphenylphosphine)palladium(II) chloride are added, the mixture is again evacuated and flushed argon. The reaction mixture is stirred at 80° C. for 16 hours. The reaction mixture is diluted with dichloromethane and water and filtered through Celite. The organic phase is separated off, washed with water again, the organic phase is dried over sodium sulfate and evaporated to dryness. The residue is recrystallised from isopropanol; yield: 2.74 g, LCMS: 366 (M+H).

1. customThe reaction mixture is evacuated twice
2. customflushed with argon
3. customthe mixture is again evacuated
4. customflushed argon
5. additionThe reaction mixture is diluted with dichloromethane and water
6. filtrationfiltered through Celite
7. customThe organic phase is separated off
8. washwashed with water again
9. dry with materialthe organic phase is dried over sodium sulfate
10. customevaporated to dryness
11. customThe residue is recrystallised from isopropanol