反应详情

温度

85 °C

To a suspension of 2,6-dibromo-4-methoxy-pyridine (5.90 g, 22.1 mmol) in DME (60 mL) and 2 M aq. K2CO3-solution (20 mL), 2,4,6-trivinylcyclotriboroxane pyridine complex (3.19 g, 13.2 mmol) is added and the mixture is degassed and put under N2 before Pd(PPh3)4 (460 mg, 0.398 mmol) is added. The mixture is stirred at 85° C. for 2 h before it is again cooled to rt, diluted with water and extracted with EA. The org. extract is dried over MgSO4, filtered and concentrated. The crude product is purified by CC on silica gel eluting with heptane:EA 4:1 to give 2-bromo-4-methoxy-6-vinyl-pyridine (4.50 g) as a yellow solid; LC-MS: tR=0.90 min, [M+1]+=213.83.

1. additionis added
2. customthe mixture is degassed
3. additionis added
4. temperatureis again cooled to rt
5. extractionextracted with EA
6. extractionextract
7. dry with materialis dried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. customThe crude product is purified by CC on silica gel eluting with heptane:EA 4:1