反应详情

温度

100 °C

To a 1000 mL round bottom flask equipped with a stirbar was added dibromopyridine 7C (22.506 g), boronic acid 7B (22.356 g), tetrakis(triphenylphosphine)palladium(0) (3.294 g), saturated sodium carbonate solution (238 mL), and toluene (190 mL). A reflux condenser was attached and the reaction was heated at 100° C. for 24 hours. The cooled reaction mixture was extracted with 1:1 hexane:ethyl acetate, and the combined organic layers were washed with brine and dried over magnesium sulfate and the solvent was removed in vacuo. The solid product was dissolved in dichloromethane, placed on silica gel, and silica gel filtered. The elution solvents were hexane, which removed a higher Rf side product, and 2.5% E/H, resulting in 31.251 g of solid. The product was recrystallized from acetonitrile to give 30.125 g of a white solid.

1. customTo a 1000 mL round bottom flask equipped with a stirbar
2. customA reflux condenser was attached
3. customThe cooled reaction mixture
4. extractionwas extracted with 1:1 hexane
5. washethyl acetate, and the combined organic layers were washed with brine
6. dry with materialdried over magnesium sulfate
7. customthe solvent was removed in vacuo
8. dissolutionThe solid product was dissolved in dichloromethane
9. filtrationfiltered
10. customremoved a higher Rf side product, and 2.5% E/H