反应详情

温度

20 °C

A solution of 4-trifluoromethoxyphenylacetonitrile (38.9 g) and 1,3-dibromopropane (39.1 g) in tetrahydrofuran (50 ml) was added under argon to a stirred solution of 50% sodium hydride (19.2 g) in tetrahydrofuran (200 ml) and dimethylformamide (25 ml) at 25°-30° C. over 1 hour. The mixture was stirred at 20° C. for 1.5 hours, then at 30°-40° C. for 1 hour, then cooled and water added. The mixture was filtered and washed with ether. The organic layer was washed with water, dried over magnesium sulphate and the solvent removed by evaporation. The residue was distilled (b.p. 111°-117° C./10 mbar) to give 1-(4-trifluoromethoxyphenyl)cyclobutanecarbonitrile (30.98 g).

1. waitat 30°-40° C. for 1 hour
2. temperaturecooled
3. filtrationThe mixture was filtered
4. washwashed with ether
5. washThe organic layer was washed with water
6. dry with materialdried over magnesium sulphate
7. customthe solvent removed by evaporation
8. distillationThe residue was distilled (b.p. 111°-117° C./10 mbar)