反应详情

温度

80 °C

1-(3-Bromophenyl)-1-(1-trityl-1H-imidazol-4-yl)-2-methyl-1-propanol (1.70 g) and a solution of tri-n-butyl(2-thienyl)tin (1.31 ml) in DMF (10 ml) were deaerated and tetrakis(triphenylphosphine)palladium(0) (110 mg) was added. The mixture was stirred under an argon atmosphere at 80° C. for 4 h. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate, washed twice with water and then with saturated brine, and dried. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chomatography (eluent, hexane:ethyl acetate=6:1→3:1). Recrystallization from ethyl acetate-hexane gave the title compound (1.32 g) as colorless powder crystals.

1. extractionthe mixture was extracted with ethyl acetate
2. washwashed twice with water
3. dry with materialwith saturated brine, and dried
4. customThe solvent was evaporated under reduced pressure
5. customthe residue was purified by silica gel column chomatography (eluent, hexane:ethyl acetate=6:1→3:1)
6. customRecrystallization from ethyl acetate-hexane