反应详情

温度

122 °C

A mixture of piperazine (Aldrich; 3.99 g), 2,4-difluorobenzonitrile, and N,N-dimethylacetamide (20 mL) is stirred for 1.5 h at 122° C. After cooling, the mixture is partitioned between dichloromethane and satd. aq. sodium bicarbonate. The organic layers are dried over magnesium sulfate and concentrated. The residue is chromatographed on silica gel and the appropriate fractions are combined and concentrated to give 1.44 g of 1-(2-cyano-5-fluorophenyl)piperazine; 1H NMR (CDCl3) δ3.01, 3.30, 6.56, 6.63, 7.40.

1. temperatureAfter cooling
2. customthe mixture is partitioned between dichloromethane
3. dry with materialThe organic layers are dried over magnesium sulfate
4. concentrationconcentrated
5. customThe residue is chromatographed on silica gel
6. concentrationconcentrated