反应详情

温度

60 °C

To a stirred solution of 2-aminopyridine (8.7 g, Aldrich) in DMF (75 mL) was added potassium hydride (12.6 g, 30 wt. % dispersion in mineral oil, Aldrich). After 1 hr, 4-bromobutyronitrile (15 g, Aldrich) was added. The mixture was heated to 60° C. for 16 hr. The mixture was quenched with water and the volatiles were removed in vacuo. The residue was extracted with ethyl acetate. The extract was filtered through a bed of silica gel and distilled in vacuo. The fraction boiling at 150° C. to 170° C. was collected to provide the title product as a white solid. 1H (CDCl3) δ 1.78 (4H, m); 2.41 (2H, t); 3.36 (2H, q); 4.53 (2H, broad t); 6.38 (1H, dt); 6.57 (1H, ddd); 7.42 (1H, ddd); 8.08 (1H, ddd). Step 2 (Alternate Procedure to Step 3, EXAMPLE A)

1. customThe mixture was quenched with water
2. customthe volatiles were removed in vacuo
3. extractionThe residue was extracted with ethyl acetate
4. filtrationThe extract was filtered through a bed of silica gel
5. distillationdistilled in vacuo
6. customThe fraction boiling at 150° C. to 170° C. was collected