反应详情

温度

80 °C

Dissolve (2-bromo-pyridin-3-yl)-(2-chloro-phenyl)-methanone (148 mg, 0.50 mmol) and 1-(3,5-bis-trifluoromethyl-benzyl)-5-methyl-4-tributylstannanyl-1H-[1,2,3]triazole (449 mg, 0.75 mmol) in DMF (5 mL) and degass, then add dichlorobis(triphenylphosphine) palladium (70 mg, 0.10 mmol). Seal the mixture under N2 and heat at 80° C. for 24 hours. Concentrate, dissolve in CHCl3, wash with saturated potassium fluoride solution (2×), saturated potassium bicarbonate solution, brine, dry over MgSO4 and concentrate. Purify the residue by flash chromatography on silica gel eluting with 0-40% EtOAc/hexane followed by recrystallization from EtOAc/hexane to afford the title compound (142 mg, 54%). MS(IS) 525 (M+1); TLC (60% EtOAc/hexane) Rf=0.30.

1. customdegass
2. customSeal the mixture under N2
3. concentrationConcentrate
4. dissolutiondissolve in CHCl3
5. washwash with saturated potassium fluoride solution (2×), saturated potassium bicarbonate solution, brine
6. dry with materialdry over MgSO4
7. concentrationconcentrate
8. customPurify the residue by flash chromatography on silica gel eluting with 0-40% EtOAc/hexane
9. customfollowed by recrystallization from EtOAc/hexane