反应详情

To a solution consisting of 40 parts of α-cyano-3-oxo-1-cyclohexen-1-acetamide in 125 parts by volume of dimethylformamide, in an atmosphere of nitrogen, is added dropwise, over a period of 10-15 minutes, 40 parts of dimethylformamide diethyl acetal. After the reaction mixture is stirred at room temperature for about 18 hours, 10 parts of water is added and the organic solvents are removed by distillation under reduced pressure. The residual oily product is extracted with dilute aqueous sodium hydroxide and the extract is washed several times with chloroform, then filtered to remove the small amount of insoluble material. Neutralization of the alkaline solution by the addition of dilute hydrochloric acid results in precipitation of the product, which is purified by recrystallization from aqueous acetone to afford 2,3,5,6,7,8-hexahydro-3,8-dioxo-4-isoquinolinecarbonitrile, melting above 290°.

1. additionis added dropwise, over a period of 10-15 minutes
2. customthe organic solvents are removed by distillation under reduced pressure
3. extractionThe residual oily product is extracted with dilute aqueous sodium hydroxide
4. washthe extract is washed several times with chloroform
5. filtrationfiltered
6. customto remove the small amount of insoluble material
7. additionNeutralization of the alkaline solution by the addition of dilute hydrochloric acid
8. customresults in precipitation of the product, which
9. customis purified by recrystallization from aqueous acetone