反应详情

温度

0 °C

To a solution of commercially available 2-amino-3-cyanopyridine (15 g, 126 mmol) in ethanol (250 mL) at 0° C. was dropwise added bromine (6.7 mL, 130 mmol) and the mixture was stirred at 0° C. for 2 h, then at 23° C. for 16 h. The solvent was totally evaporated, water (200 mL) was added, then sat. NaHCO3-solution until neutral. Extracted with AcOEt (3×300 mL), the organic layer was dried over Na2SO4, filtered and totally evaporated. The residue was triturated with ether to give the title compound as a light yellow solid (23.5 g, 94%). MS (ISP) 198.1 [(M+H)+], 200.2 [(M+2+H)+].

1. customat 0° C.
2. waitat 23° C. for 16 h
3. customThe solvent was totally evaporated
4. additionwater (200 mL) was added
5. extractionExtracted with AcOEt (3×300 mL)
6. dry with materialthe organic layer was dried over Na2SO4
7. filtrationfiltered
8. customtotally evaporated
9. customThe residue was triturated with ether