反应详情

A solution of 3-bromo-2-cyanopyridine (Chem. Pharm. Bull, 1985, 33, 565) (2.6 g, 14.2 mmol) and sodium azide (1.0 g, 15.3 mmol) in DMF (30 ml) was heated at 90° C. for 16 h. The resulting mixture was cooled, water was added and the whole was extracted with ethyl acetate. The combined extracts were washed with saturated brine and dried over magnesium sulphate. Evaporation of the solvent gave the product as an oil, which was purified by flash column chromatography on silica gel, eluting with ethyl acetate/petrol (1:3 to 1:1) as eluent to afford the product. MS (EI) m/z 145; 1H NMR (d6-DMSO) 8.50 (1H, d), 8.09 (1H, d), 7.77 (1H, dd).

1. temperatureThe resulting mixture was cooled
2. extractionthe whole was extracted with ethyl acetate
3. washThe combined extracts were washed with saturated brine
4. dry with materialdried over magnesium sulphate
5. customEvaporation of the solvent