反应详情

A solution of 4-bromo-3-fluorophenylacetonitrile (5 g, 23 mmoles) in toluene (20 ml) is added with 35 mmoles of 1,2-dibromoethane, a 50% NaOH aqueous solution (20 ml) and tetrabutylammonium bromide (1.6 g, 5 mmoles). The mixture is kept under stirring at room temperature for 5-12 hours, then diluted with water and extracted with ethyl acetate. The organic phase is washed with 1N HCl, then with brine, finally dried and concentrated under vacuum to give a brown solid, which is subjected to chromatography on a silica gel column (200 g), eluting with hexane-ethyl ether 1-1, to afford the product in the solid form.

1. extractionextracted with ethyl acetate
2. washThe organic phase is washed with 1N HCl
3. dry with materialwith brine, finally dried
4. concentrationconcentrated under vacuum
5. customto give a brown solid, which
6. washeluting with hexane-ethyl ether 1-1
7. customto afford the product in the solid form