HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 2,3,4,5-Tetrahydro-1,4-benzoxazepine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 4,5-dihydro-1,4-benzoxazepin-3(2H)-one | HCID 919801 | — |
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 2,3,4,5-Tetrahydro-1,4-benzoxazepine | HCID 21882775 | 90,5% |
Reaktionsschritte
To the suspension of lithium aluminium hydride (15.2 g, 0.4 mol) in 600 mL of ether was added a solution of 4,5-dihydro-1,4-benzoxazepin-3(2H)-one (16.3 g, 0.1 mol) in 60 mL of tetrahydrofuran at room temperature. After being heated with stirring under reflux overnight, water was added dropwise to quench the reaction at 0° C., The resulting mixture was diluted with ethyl acetate, and then filtered by a pad of celite. The filtrate was concentrated under reduced pressure, followed by the addition of hydrochloric acid ethyl acetate solution. The hydrochloride was collected by filtration, washed with ethyl acetate then ether, and then dried in vacuo to give 13.5 g of product. MS obsd. (ESI+) [(M+H)+] 150.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08871756B2 |
| Quelldatensatz | uspto-grants-2014_10 |
| ORD ID | ord-211d2f2e0fba4bb7af15e05910860a84 |
| Quellennotiz | uspto-grants-2014_10 |