HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 1,2,3,4,5,6-Hexahydro-3,9-dimethylazepino[4,5-b]indole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | 4-Methylphenylhydrazine monohydrochloride | HCID 12504 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 1-Methylazepan-4-one | HCID 262586 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 1,2,3,4,5,6-Hexahydro-3,9-dimethylazepino[4,5-b]indole | HCID 68560092 | — |
Reaktionsschritte
The title compound was prepared by following general procedure 1. p-Tolyl hydrazine hydrochloride (15 g, 94.55 mmol) was taken into 7% H2SO4 in 1,4-dioxane (650 mL), 1-methylazepan-4-one.HCl (15.4 g, 94.55 mmol) was added and stirred at RT for 10 min. The reaction mixture was stirred at 80° C. for 14 h. After completion of the reaction, reaction mass was slowly basified with 50% NaOH solution, extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and evaporated to dryness and purified by column chromatography (silica gel 100-200 mesh; eluent: 10% methanol-DCM) to afford 3,9-dimethyl-1,2,3,4,5,6-hexahydroazepino[4,5-b]indole (5 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08569287B2 |
| Quelldatensatz | uspto-grants-2013_10 |
| ORD ID | ord-b22701505ed14544a4d9467fc8af3208 |
| Quellennotiz | uspto-grants-2013_10 |