HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrazinium chloride → HCID 178469860, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrazinium chloride | HCID 115031 | — |
| Edukt | 1-Tert-butyl 3-ethyl 5-((dimethylamino)methylene)-4-oxopiperidine-1,3-dicarboxylate | HCID 68465860 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | HCID 178469860 | HCID 178469860 | — |
Reaktionsschritte
A solution of enaminoketone 3b (327 mg, 1.00 mmol) in abs. EtOH (10 mL) was cooled to 0° C. and hydrazine monohydrogen chloride was added in one portion. The mixture was stirred for 18 h during which time the temperature reached rt after 2 h. The mixture was concentrated and the residue partitioned with deionized H2O and EtOAc. The organic layer was removed and the aqueous portion extracted with EtOAc (2×). The combined EtOAc portions were washed with brine, dried over MgSO4 and filtered through a SiO2 plug capped with a MgSO4 layer (EtOAc for elution). The solution was concentrated give the title compound 4b as a brittle white foam crushed to a white solid; 253 mg, 87%, MS m/z 240.0, 194.0 (ESI+, M−tBu, M−Boc).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07781474B2 |
| Quelldatensatz | uspto-grants-2010_08 |
| ORD ID | ord-78ff8f8c81bd4e489a8e338a8c6bb5c4 |
| Quellennotiz | uspto-grants-2010_08 |