HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 7-Bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Ethanol | HCID 702 | — |
| Edukt | 1,4-Dioxane | HCID 31275 | — |
| Edukt | tert-Butyl 7-bromo-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate | HCID 25220760 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | 7-Bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride | HCID 66820137 | 98% |
Reaktionsschritte
1,1-dimethylethyl 7-bromo-2,3-dihydro-1,4-benzoxazepine-4 (5H)-carboxylate (10 g, 30.5 mmol) was taken into hot ethanol (10 mL) followed by addition of 4M hydrogen chloride in dioxane solution (2.1 eq, 16 mL) and the resulting solution was allowed to slowly cool to ambient temperature over one hour. An excess of ethyl ether was then added and the resulting slurry was filtered. The filter cake was washed with ethyl ether and dried to give 7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride (7.9 g, 98% yield) as a colorless crystalline solid. MS (EI) for C9H10NOBr: 229 (MH+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08637499B2 |
| Quelldatensatz | uspto-grants-2014_01 |
| ORD ID | ord-3d1c6b8d66da4b39b979a793961ed21b |
| Quellennotiz | uspto-grants-2014_01 |