HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → 4-[3-(Trifluoroacetylamino)propylthio]pyridine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-(3-Aminopropylthio)pyridine dihydrochloride | HCID 19079259 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-[3-(Trifluoroacetylamino)propylthio]pyridine hydrochloride | HCID 19079263 | 68.4% |
Reaction Steps
To a solution of 1.00 g (4.15 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 2.77 ml (19.8 mmol) of triethylamine in 40 ml of methylene chloride was added 0.70 ml (4.96 mmol) of anhydrous trifluoroacetic acid under ice-cooling with stirring and the mixture was stirred for at room temperature for 30 minutes. The reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water and dried. The solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate ) to obtain the powder which was washed with hexane and dried to obtain 750 mg of the desired compound (free base) (68.4%, pale yellow prisms).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05246948 |
| Source dataset | uspto-grants-1993_09 |
| ORD ID | ord-657feb5cd33641b8bf5a3da5d5b2469f |
| Source note | uspto-grants-1993_09 |