反应详情

A mixture of 1.63 g potassium cyanide and 8 g of the compound from Example 1 in 50 ml of DMSO was stirred at room temperature overnight. The solution became darker in color with time, going from orange to purple to black. After being stirred overnight the reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried (MgSO4), filtered and the solvent evaporated. The residual red oil was eluted through a dry silica column with 20% ethyl acetate--80% dichloromethane. The product band was isolated to give 3.0 g solid m.p. 146°-147° C.;

1. stirringAfter being stirred overnight the reaction mixture
2. customwas partitioned between ethyl acetate and water
3. washThe organic layer was washed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customthe solvent evaporated
7. washThe residual red oil was eluted through a dry silica column with 20% ethyl acetate--80% dichloromethane
8. customThe product band was isolated