HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 1,4-Dihydro-1-phenylindeno[1,2-c]pyrazole
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Phenylhydrazine hydrochloride | HCID 60962 | — |
| Edukt | 1H-Inden-1-one, 2,3-dihydro-2-(hydroxymethylene)- | HCID 3764882 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 1,4-Dihydro-1-phenylindeno[1,2-c]pyrazole | HCID 10879009 | — |
Reaktionsschritte
2-Hydroxymethlene indan-1-one (Example 1(ii)(a) (6.0 g, 37.5 mmol), phenylhydrazine hydrochloride (Aldrich) (5.48 g, 37.9 mmol), 10 M hydrochloric acid (1 cm3) and ethanol (30 cm3) were stirred under reflux for 19 hours. After cooling, the solvent was evaporated under reduced pressure and the residue dissolved in dichloromethane, then washed with 2M sodium hydroxide. The organic layer was separated, dried (Na2SO4) filtered and concentrated in vacuo. Purification by Kugelrohr distillation afforded an off-white solid (150° C., 0.01 mmHg) m.p. 119-120° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06130228 |
| Quelldatensatz | uspto-grants-2000_10 |
| ORD ID | ord-380d35a1d5e1462b8e71bdae12a790df |
| Quellennotiz | uspto-grants-2000_10 |