HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonia → 8-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | Potassium Nitrate | HCID 24434 | — |
| Edukt | 2,3,4,5-tetrahydro-1H-1-benzazepine | HCID 576503 | — |
| Lösungsmittel | Sulfuric Acid | HCID 1118 | — |
| Produkt | 8-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine | HCID 46864071 | 52% |
Reaktionsschritte
At −10° C., 2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.9 g, 13 mmol) was added dropwise to a solution of KNO3 (3 g, 30 mmol) in H2SO4 (50 mL). The mixture was stirred for 40 min, poured over crushed ice, basified with aq. ammonia to pH 13, and extracted with EtOAc. The combined organic phases were washed with brine, dried over Na2SO4 and concentrated to give 8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine as a black solid (1.3 g, 51%), which was used without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08101767B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-df8129f99fb94400af951e60a4e601ac |
| Quellennotiz | uspto-grants-2012_01 |