反应详情

To a solution of ethyl 2-amino-2-cyanoacetate (1 eq) in 6 mL of dichloromethane was added pyridine (1.5 eq) and 2,6-difluorobenzoyl chloride (1 eq) at 0° C. The reaction mixture was stirred at room temperature for 3 hours. The mixture was diluted with ethyl acetate, washed with brine, then dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The crude residue was purified by flash chromatography (EtOAc:hexanes=1:1) to give the titled compound (84%). LC/MS (m/z): 269.1 (MH+), Rt:0.69 min.

1. washwashed with brine
2. dry with materialdried over anhydrous MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude residue was purified by flash chromatography (EtOAc:hexanes=1:1)