反应详情

A mixture of 6-amino-3-bromo-2-methylpyridine (20.0 g, 0.107 mol)(Maybridge) and copper (I) cyanide 11.0 g, 0.123 mol) in DMF (25 ml) was heated to reflux for 4 h. The DMF was evaporated in vacuo and the residue was partitioned between ethyl acetate and 10% sodium cyanide solution. The organic layer was washed with 10% sodium cyanide solution and brine, dried (Na2SO4) and evaporated in vacuo to a brown solid. This was dissolved in a minimum amount of ethyl acetate and the product was precipitated by adding hexanes. The mixture was filtered to give the title compound as a brown powder:

1. temperaturewas heated
2. temperatureto reflux for 4 h
3. customThe DMF was evaporated in vacuo
4. customthe residue was partitioned between ethyl acetate and 10% sodium cyanide solution
5. washThe organic layer was washed with 10% sodium cyanide solution and brine
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo to a brown solid
8. dissolutionThis was dissolved in a minimum amount of ethyl acetate
9. customthe product was precipitated
10. additionby adding hexanes
11. filtrationThe mixture was filtered