反应详情

Place 4-bromopyridine hydrochloride (2.33 g, 12 mmol), α-(ethynyl)-benzenemethanol (1.95 g, 14.8 mmol) and diethylamine (25 mL) under nitrogen atmosphere. Add bis(triphenylphosphine)palladium(II) chloride (105 mg) then copper(I) iodide (59 mg). Stir at room temperature for 3 hours. Evaporate the solvent in vacuo, stir the residue in ethyl acetate (50 mL) and filter the solids. Evaporate the solvent in vacuo and purify by silica gel chromatography (4:3 ethyl acetate/hexane) to yield 0.4 g. Recrystallize (hexane/chloroform) to yield 0.2 g of the title compound; mp 93°-96° C.

1. customEvaporate the solvent in vacuo
2. stirringstir the residue in ethyl acetate (50 mL)
3. filtrationfilter the solids
4. customEvaporate the solvent in vacuo
5. custompurify by silica gel chromatography (4:3 ethyl acetate/hexane)
6. customto yield 0.4 g
7. customRecrystallize (hexane/chloroform)