反应详情

To a solution of 4.0 g (10 mmol) of the product of Example 10 in 60 mL of pyridi was added 2.0 g (22 mmol) of copper (I) cyanide and the resulting mixture was refluxed for 48 h. The reaction mixture was then cooled to room temperature, poured over cold water, stirred for 16 h and then carefully acidified with concentrated HCl solution. The resulting solid was filtered and washed with water, dissolved in chloroform, dried over MgSO4, filtered and concentrated in vacuo. The residue was triturated with ether, filtered and dried to provide 2.0 g (58%) of the desired product as a white solid. m.p. 175° C.; Electrospray Mass Spec 347 (M+H).

1. temperaturethe resulting mixture was refluxed for 48 h
2. filtrationThe resulting solid was filtered
3. washwashed with water
4. dissolutiondissolved in chloroform
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe residue was triturated with ether
9. filtrationfiltered
10. customdried