反应详情

温度

100 °C

4-Fluorobenzonitrile (6.0 g, 49.5 mmol) was dissolved in acetonitrile (60 ml), and benzylamine (10.6 g, 98.9 mmol) was added thereto, followed by stirring at 100° C. for 3 days. To complete the reaction, benzylamine (21.2 g, 198 mmol) was further added thereto, followed by stirring at 100° C. for 1 day. The solvent was removed under reduced pressure, water was added to the resulting residue, and the mixture was extracted with chloroform. After the organic layer was dried (over anhydrous magnesium sulfate), the drying agent was filtered off, and the filtrate was concentrated under reduced pressure. The resulting oily substances were purified by silica gel column chromatography (the substances were eluted with an increasing concentration of chloroform from chloroform/hexane=1/2 to chloroform/hexane=1/1) to give the title compound (7.42 g, 72%) as oily substances.

1. additionwas further added
2. stirringby stirring at 100° C. for 1 day
3. customThe solvent was removed under reduced pressure, water
4. additionwas added to the resulting residue
5. extractionthe mixture was extracted with chloroform
6. dry with materialAfter the organic layer was dried (over anhydrous magnesium sulfate)
7. filtrationthe drying agent was filtered off
8. concentrationthe filtrate was concentrated under reduced pressure
9. customThe resulting oily substances were purified by silica gel column chromatography (the substances
10. washwere eluted with an increasing concentration of chloroform from chloroform/hexane=1/2 to chloroform/hexane=1/1)