反应详情

温度

90 °C

A mixture of 4-(4,4,5,5-Tetramethyl[1,3,2]dioxaborolan-2-yl)-1H-pyrazole (5.0 g, 0.026 mol), 2-bromo-2-methylpropionic acid methyl ester (3.50 mL, 0.0270 mol), Cs2CO3 (12 g, 39 mmol) in DMF (200 mL) was heated at 90° C. overnight. Reaction mixture was concentrated in vacuo, water was added, and the mixture was extracted with EtOAc (3×50 mL). The organic layer was dried over Na2SO4 and concentrated in vacuo to afford the title compound as a light yellow solid. MS (ES+): m/z 295.13, 296.16 (100, 50) [MH+]. HPLC: tR=3.35 min (ZQ3 polar—5 min).

1. customReaction mixture
2. concentrationwas concentrated in vacuo, water
3. additionwas added
4. extractionthe mixture was extracted with EtOAc (3×50 mL)
5. dry with materialThe organic layer was dried over Na2SO4
6. concentrationconcentrated in vacuo