HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonium Hydroxide → 2,3,4,5-tetrahydro-1H-1,5-benzodiazepine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonium Hydroxide | HCID 14923 | — |
| Edukt | 2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one | HCID 223771 | — |
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 2,3,4,5-tetrahydro-1H-1,5-benzodiazepine | HCID 577192 | — |
Reaktionsschritte
To an ice cold solution of lithium aluminium hydride (4.68 g, 123 mmol) in dry THF (100 ml), under a nitrogen atmosphere, was added dropwise a solution of 2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-2-one (5.0 g, 30.9 mmol) in dry THF (50 ml). The mixture was allowed to warm to room temperature and then heated at reflux for 2 h. The mixture was then cooled to 0° C. and a solution of aqueous ammonium hydroxide (10 ml) in THF (60 ml) was added dropwise. The resultant suspension was stirred for 1 h and then filtered through a pad of celite. The filtrate was evaporated in vacuo to give a tan solid; yield 4.36 g (95%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07176195B2 |
| Quelldatensatz | uspto-grants-2007_02 |
| ORD ID | ord-4f35f10ec4584bbfb6354bb9f3a5e6b1 |
| Quellennotiz | uspto-grants-2007_02 |