反应详情

To a solution of 25.3 g of potassium cyanide in 100 ml of water is added 400 ml of methanol and to the solution is added 41 g of 5-dimethylaminomethyl-5,6-dihydro-4H-thieno[2,3-b]thiopyran-4-one hydrochloride with stirring. The mixture is stirred for 3 hours at 45°-50° C. and then concentrated under reduced pressure. To the residue is added water and the mixture is extracted with chloroform. The extract is washed with water, dried over magnesium sulfate and the chloroform is distilled off. The residue is subjected to chromatography on silica gel and eluted with chloroform to give 28 g of 4-oxo-5,6-dihydro-4H-thieno[2,3-b]thiopyran-5-acetonitrile as pale brown oil.

1. stirringThe mixture is stirred for 3 hours at 45°-50° C.
2. concentrationconcentrated under reduced pressure
3. additionTo the residue is added water
4. extractionthe mixture is extracted with chloroform
5. washThe extract is washed with water
6. dry with materialdried over magnesium sulfate
7. distillationthe chloroform is distilled off
8. washeluted with chloroform