反应详情

温度

80 °C

A slurry of N-[(p-chlorophenyl)cyanomethyl]-2,2,2-trifluoroacetamide (13.1 g, 0.05 mol) in toluene is treated sequentially with methanesulfonic acid (2.4 g, 0.025 mol) and acetyl chloride (4.32 g, 0.055 mol), at room temperature, heated at 80° C. for 2 hours, cooled to room temperature, diluted with acetonitrile, treated first with 2-chloroacrylonitrile (5.25 g, 0.06 mol) then dropwise with triethylamine (13.7 g, 0.135 mol), heated at 70°-72° C. for 1 hour, cooledto room temperature and diluted with water. The mixture is extracted with ethyl acetate. The extracts are combined, washed with water and concentrated in vacuo to give a residue. Flash chromatography (silica-gel;15% ethylacetate in heptane as eluent) gives the title product.

1. temperaturecooled to room temperature
2. customcooledto room temperature
3. extractionThe mixture is extracted with ethyl acetate
4. washwashed with water
5. concentrationconcentrated in vacuo
6. customto give a residue