反应详情

温度

100 °C

A mixture of DME: H2O (3:1) was degassed with N2 for one half hour. 2-bromo-1-chloro-4-nitrobenzene (1 eq) added and degassed for another 10 minutes. 1,1′-bis(diphenylphosphino)ferrocene palladium(II)chloride (0.05 eq), 3-fluoropyridin-4-yl-4-boronic acid (1 eq), and sodium carbonate (3 eq) were then added and stirred at 100° C. for 16 hours. Reaction then concentrated and partitioned between ethyl acetate and water. Organic layer washed with brine, dried over sodium sulfate and concentrated. Purification on silica gel, 10% ethyl acetate in hexanes to yield 4-(2-chloro-5-nitrophenyl)-3-fluoropyridine. HPLC=4.57 min; MS: MH+=253.

1. customwas degassed with N2 for one half hour
2. customdegassed for another 10 minutes
3. customReaction
4. concentrationthen concentrated
5. custompartitioned between ethyl acetate and water
6. washOrganic layer washed with brine
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated
9. customPurification on silica gel, 10% ethyl acetate in hexanes