反应详情

Potassium hexamethyldisilazide (0.5 mol/L in toluene, 34 mL) was added over a period of 5 min to a solution of 5-bromo-2-fluoro-pyridine (1.50 g) and cyclopropanecarbonitrile (0.63 mL) in toluene (2 mL) chilled in an ice bath. Aqueous NH4Cl solution was then added and the resulting mixture was extracted with ethyl acetate. The combined extracts were dried (Na2SO4) and the solvent was evaporated. The residue was chromatographed on silica gel (cyclohexane/ethyl acetate 1:0→8:2) to give the title compound as a colorless solid. Yield: 0.19 g (10% of theory); LC (method 2): tR=3.34 min; Mass spectrum (ESI+): m/z=223/225 (Br) [M+H]+.

1. temperaturechilled in an ice bath
2. extractionthe resulting mixture was extracted with ethyl acetate
3. dry with materialThe combined extracts were dried (Na2SO4)
4. customthe solvent was evaporated
5. customThe residue was chromatographed on silica gel (cyclohexane/ethyl acetate 1:0→8:2)