HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 20430559, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 12751998 | HCID 12751998 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Product | HCID 20430559 | HCID 20430559 | 72% |
Reaction Steps
A solution of 7-oxo-5-tosyl-4,5,6,7-tetrahydro-thieno[3,2-c]pyridine (19.6 g; 0.064 mole; obtained in (b) above) and potassium tert-butoxide (28.6 g; 0.255 mole) in tert-butanol (300 ml) is refluxed for 2 hours under a nitrogen atmosphere. Evaporation of the solvent in vacuo leaves a residue which is taken up into 2N hydrochloric acid. The aqueous phase is extracted with ether, made basic by addition of concentrated ammonia, and evaporated to dryness. The residue is extracted four times with boiling ethyl acetate. The organic extracts are filtered through a silica bed and evaporated to dryness. The solid residue is recrystallized from ethanol-acetonitrile. Greyish crystals; M.P.=180° C.; Yield: 72%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04496568 |
| Source dataset | uspto-grants-1985_01 |
| ORD ID | ord-4e2e22798c1045feb3ba95a9bf93cf75 |
| Source note | uspto-grants-1985_01 |