反应详情

To a mixture of 3,5-difluoro-phenylacetonitrile (11.48 g), 1,2-dibromoethane (42.2 ml) and benzyltriethylammonium chloride (0.68 g) was added sodium hydroxide solution (50% in water, 30 ml) at room temperature. The mixture was vigorously stirred overnight. Water was added and the aqueous phase was extracted twice with diethyl ether. The combined organic layers were washed with water and brine, dried over MgSO4 and concentrated. The residue was purified by column chromatography (SiO2; heptane/EtOAc) to give 1-(3,5-difluoro-phenyl)cyclopropanecarbonitrile as a light pink solid (8.23 g). 1H-NMR (300 MHz, CDCl3, δ): 1.40-1.44, (m, 2H), 1.78-1.82 (m, 2H), 6.70-6.85 (m, 3H).

1. extractionthe aqueous phase was extracted twice with diethyl ether
2. washThe combined organic layers were washed with water and brine
3. dry with materialdried over MgSO4
4. concentrationconcentrated
5. customThe residue was purified by column chromatography (SiO2; heptane/EtOAc)