HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → tert-Butyl (3R)-3-(aminomethyl)piperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | (S)-Tert-butyl 3-(azidomethyl)piperidine-1-carboxylate | HCID 10083012 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | tert-Butyl (3R)-3-(aminomethyl)piperidine-1-carboxylate | HCID 1502023 | 92.9% |
Reaction Steps
To a solution of 600 mg of (3S)-3-azidomethyl-1-(tert-butoxycarbonyl)piperidine in 12.5 ml of 20% hydrous tetrahydrofuran, 622 mg of triphenylphosphine was added at room temperature, followed by 45 minutes' refluxing under heating. The reaction liquid was rendered acidic by addition of 0.5 N hydrochloric acid, and successively washed with chloroform and ethyl acetate. Then 4N aqueous sodium hydroxide solution was added to the aqueous layer to render the latter basic, followed by extraction with chloroform and drying over anhydrous sodium sulfate. Distilling the solvent off under reduced pressure, 497 mg of the title compound was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06809108B1 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-963f4bc1c8c8429fb5a34c9a88126b4a |
| Source note | uspto-grants-2004_10 |