HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 20239761, compound → HCID 13281205, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 20239761 | HCID 20239761 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 13281205 | HCID 13281205 | 62.4% |
Reaction Steps
A mixture of hexahydro-4-[2-(1H-imidazol-1-yl)ethyl]-1H-azepine-carboxaldehyde (11 g, 0.05M) in dioxane (1.65 ml) and 2N HCl (82 ml) was heated and refluxed for 15 hrs. The solvent was removed, water (100 ml) was added and the resulting mixture was washed with methylene chloride (3×20 ml). After washing, the aqueous solution was basified with 4N NaOH to pH 12 and extracted with methylene chloride (4×75 ml). The combined extracts, dried over sodium sulfate, were stripped to yield hexahydro-4-[2-(1H-imidazol-1-yl)ethyl]-1H-azepine as an oil (6 g, 62% yield). This compound was characterized as dihydrochloride salt m.p. 176°-177° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04537969 |
| Source dataset | uspto-grants-1985_08 |
| ORD ID | ord-03fb48d729d448d19352853fb32f7dc2 |
| Source note | uspto-grants-1985_08 |