HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 4-oxo-5,6-dihydro-4H-thieno[2,3-b]thiopyran-5-acetonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Potassium Cyanide | HCID 9032 | — |
| Reactant | 5-dimethylaminomethyl-5,6-dihydro-4H-thieno[2,3-b]thiopyran-4-one hydrochloride | HCID 12675307 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-oxo-5,6-dihydro-4H-thieno[2,3-b]thiopyran-5-acetonitrile | HCID 15225034 | 86.1% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05329016 |
| Source dataset | uspto-grants-1994_07 |
| ORD ID | ord-c3a7215459c6468fa80c4fe1aeae4247 |
| Source note | uspto-grants-1994_07 |