HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl 4-chloro-5-cyano-2,3,6,7-tetrahydro-1H-azepine-1-carboxylate → 4-Chloro-5-cyano-2,3,6,7-tetrahydro-1H-azepine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl 4-chloro-5-cyano-2,3,6,7-tetrahydro-1H-azepine-1-carboxylate | HCID 13072036 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4-Chloro-5-cyano-2,3,6,7-tetrahydro-1H-azepine hydrochloride | HCID 20481325 | — |
Reaction Steps
1.45 gm (0.005 mol) of benzyl 4-chloro-5-cyano-2,3,6,7-tetrahydro-1H-1-azepine-carboxylate were dissolved in 20 ml of ethyl alcohol by addition of 0.9 ml of semiconcentrated hydrochloric acid, and after the addition of 0.2 gm of palladium-on-charcoal, the mixture was hydrogenated in an autoclave at room temperature and under a hydrogen pressure of 5 bars. After half an hour, the uptake of hydrogen had ended. The catalyst was filtered off, and the filtrate was evaporated in vacuo. The residue was recrystallized from isopropyl alcohol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04414225 |
| Source dataset | uspto-grants-1983_11 |
| ORD ID | ord-a6fa2d10549c4504a613980442eb2a64 |
| Source note | uspto-grants-1983_11 |