反应详情

温度

65 °C

To a solution of ethyl 2-bromo-3-(3-cyanophenyl)-3-oxopropionate (1.0 g, 3.4 mmol) in 20 mL of tetrahydrofuran was added thionicotinamide (0.46 g, 3.4 mmol). The resulting mixture was stirred at 65° C. for 16 h. The reaction was allowed to cool and the solvent was evaporated in vacuo. The residue was triturated with chloroform, taken up in ethyl acetate, washed with saturated aq Na2CO3 and brine, dried (MgSO4) and concentrated in vacuo to yield a solid. Trituration with ethyl acetate left the title compound as an off-white solid (0.26 g, 23%). MS (ESI) 336.1 (M+H)+.

1. temperatureto cool
2. customthe solvent was evaporated in vacuo
3. customThe residue was triturated with chloroform
4. washwashed with saturated aq Na2CO3 and brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated in vacuo
7. customto yield a solid