反应详情

温度

65 °C

To a solution of ethyl 2-bromo-3-(3-cyanophenyl)-3-oxopropionate (4.0 g, 13.5 mmol) in 100 mL of tetrahydrofuran was added thiourea (1.03 g, 13.5 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 ether, 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 ether left the title compound as an off-white solid (3.79 g, 98%).

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