反应详情

温度

70 °C

A 50% aqueous solution of sodium hydroxide (18 g, 46 mmol) was slowly added to a mixture of (3,4-difluoro-phenyl)-acetonitrile (7.1 g, 46 mmol), benzyltriethylammonium chloride (0.26 g, 1.2 mmol) and 1-bromo-2-chloroethane (15 g, 105 mmol) at 70° C. The mixture was stirred overnight at 70° C. The cooled reaction mixture was diluted with water (50 mL) and extracted three times with ethyl acetate (50 mL). The combined organic layers were washed with a saturated aqueous solution of sodium chloride, dried over sodium sulfate, and evaporated to dryness to give crude 1-(3,4-difluoro-phenyl)-cyclopropanecarbonitrile which was used directly in the next step. 1H NMR (CDCl3): δ 7.18-7.03 (m, 3H), 1.79-1.69 (m, 2H), 1.43-1.38 (m, 2H).

1. customThe cooled reaction mixture
2. extractionextracted three times with ethyl acetate (50 mL)
3. washThe combined organic layers were washed with a saturated aqueous solution of sodium chloride
4. dry with materialdried over sodium sulfate
5. customevaporated to dryness