反应详情

温度

90 °C

To a solution of ethyl 3-(4-cyanophenyl)-2-formylpropanoate (1.3 g, 5.62 mmol) in Ethanol (60 mL) was added thiourea (1.712 g, 22.49 mmol) under argon. The mixture was heated at 90° C. for 3 h. After removing the solvent, the residue was dissolved in water (80 mL), washed with ether twice. The aqueous solution was acidified to pH 4-5 with acetic acid, and the resulting precipitate was collected by filtration, washed with water until the wash waters were neutral to afford the title compound (0.95 g, 3.90 mmol, 69.5% yield). LCMS: rt=1.86 min, [M+H+]=224

1. customAfter removing the solvent
2. dissolutionthe residue was dissolved in water (80 mL)
3. washwashed with ether twice
4. filtrationthe resulting precipitate was collected by filtration
5. washwashed with water until the wash waters