反应详情

A stirred solution of D7 (9.06 g, 26 mmole) in dry degassed DMF (150 ml) was treated with copper (I) iodide (495 mg, 2.6 mmole), dichlorobis(triphenylphosphine)palladium(II) (1.52 g, 2.2 mmole) and 4-bromopyridine (prepared by suspending the HCl salt (6.07 g, 31 mmole) in 40% KOH solution, extracting with toluene and adding the dried toluene solution to the reaction). The mixture was heated at reflux under argon for 5 h and allowed to cool before removing the DMF under vacuum. The residue was partitioned between EtOAc and 10% NaHCO3 solution and the organics dried (Na2SO4) and chromatographed on silica gel eluting with EtOAc to afford the title compound as a white solid (4.1 g, 60%).

1. customdegassed DMF (150 ml)
2. customprepared
3. extractionextracting with toluene
4. additionadding the dried toluene solution
5. customto the reaction)
6. temperatureThe mixture was heated
7. temperatureat reflux under argon for 5 h
8. temperatureto cool
9. custombefore removing the DMF under vacuum
10. customThe residue was partitioned between EtOAc and 10% NaHCO3 solution
11. dry with materialthe organics dried (Na2SO4)
12. customchromatographed on silica gel eluting with EtOAc