反应详情

98.5 g (0.5 mol) of diisopropyl-cyanoacetic acid ethyl ester (prepared according to J. Chem. Soc., 1930, page 2,758), 300 ml of 1-oxo-1-methyl-phospholine, 31 g of sodium chloride and 22 g of water were heated to 160°-170° C. for 9 hours. After cooling, the mixture was diluted with 1,000 ml of water and extracted by shaking four times with 150 ml of petroleum ether each time. The combined petroleum ether phases were washed twice with 200 ml of water each time and dried with Na2SO4 and the petroleum ether was distilled off under normal pressure. The residual crude product was then purified by vacuum distillation. 53.2 g (85% of theory) of diisopropyl-acetonitrile of boiling point 60° C./14 mm Hg were obtained. Refractive index nD20 =1.4190.

1. temperatureAfter cooling
2. extractionextracted
3. washThe combined petroleum ether phases were washed twice with 200 ml of water each time
4. dry with materialdried with Na2SO4
5. distillationthe petroleum ether was distilled off under normal pressure
6. distillationThe residual crude product was then purified by vacuum distillation