反应详情

To a stirred solution of (XII) (966 mg) in t-butanol was added 250 mg of acrylonitrile dissolved in 1 ml t-butanol over a period of 1 hour. Continued stirring for 3.5 hours at room temperature and finally refluxed for 1.5 hours. Chloroform was added and the product was extracted into 1N H2SO4. The aqueous phase was washed once with CHCl3, then basified to pH 10 with 2N NaOH and the free amine extracted into CHCl3. The product (XIII) 1.04 g was obtained by evaporation of the solvents under vacuum.

1. temperaturefinally refluxed for 1.5 hours
2. extractionthe product was extracted into 1N H2SO4
3. washThe aqueous phase was washed once with CHCl3
4. extractionthe free amine extracted into CHCl3