反应详情

A mixture of 25.4 g (179 mmol) 2,6-difluorobenzaldehyde, 19.5 ml (197 mmol) N-butylamine and 0.68 g (3.57 mmol) p-toluenesulfonic acid in 120 ml toluene was heated in a Dean-Stark apparatus at reflux for 3 hours. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate and washed sequentially with water (twice) and with saturated brine. The organic phase was dried over Na2SO4, filtered, and concentrated in vacuo to afford the title compound 30.4 g (86%) as a brown oil which was used in the next step without further purification. MS (ISP): 198.3 ([M+H]+, 100%).

1. temperaturewas heated in a Dean-Stark apparatus
2. temperatureat reflux for 3 hours
3. washwashed sequentially with water (twice) and with saturated brine
4. dry with materialThe organic phase was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo