反应详情

温度

85 °C

Water (160 mL) was added dropwise at room temperature to a mixture of 4-ethoxycarbonylphenylboronic acid (50 g, 0.26 mol), 3-bromopyrazolo[1,5-a]pyrimidine (56.25 g, 0.28 mol), Pd(ddpf)Cl2.CH2Cl2 (4.25 g, 5.21 mmol), and Cs2CO3 (169.42 g, 0.52 mol) in 1,4-dioxane (1 L). The reaction mixture was then heated 85° C. for 4 h. The reaction mixture was cooled, poured into water and extracted with EtOAc (2×300 mL). The combined organic layers were dried over Na2SO4, filtered, and the filtrate was concentrated under reduced pressure. The crude product was purified by silica gel chromatography eluting with a gradient of petroleum ether: EtOAc (100:10 to 3:1) to deliver the title compound (64 g, 93%) as a yellow solid.

1. temperatureThe reaction mixture was cooled
2. extractionextracted with EtOAc (2×300 mL)
3. dry with materialThe combined organic layers were dried over Na2SO4
4. filtrationfiltered
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe crude product was purified by silica gel chromatography
7. washeluting with a gradient of petroleum ether: EtOAc (100:10 to 3:1)