反应详情

温度

55 °C

To 19.6 g (0.1 mol) of 1-cyano-1-n-pentanoylaminocyclopentane dissolved in 70 ml of methanol, 25 g (0,46 mol) of potassium hydroxide dissolved in 50 ml of water was added. The resulting solution was stirred and heated at 50-60° C., then under reflux conditions for 2,5 hours. The pH was decreased by the addition of 25 g of ammonium chlorid, then methanol was distilled off. The residue was extracted with 50 ml and 2×30 ml of toluene, the combined organic phases were evaporated to constant weight The residual 16 g of title compound was dissolved in 100 ml of acetone, the pH of the resulting solution was adjusted to 1-2 with hydrochloric acid solution, the mixture was crystallized, the crystals were collected by filtration to obtain 14 g of the title compound, yield 60.8%.

1. additionwas added
2. waitunder reflux conditions for 2,5 hours
3. distillationmethanol was distilled off
4. extractionThe residue was extracted with 50 ml and 2×30 ml of toluene
5. customthe combined organic phases were evaporated to constant weight The residual 16 g of title compound
6. dissolutionwas dissolved in 100 ml of acetone
7. customthe mixture was crystallized
8. filtrationthe crystals were collected by filtration