HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium hydride → 2-(6,7-Dimethoxy-quinoxalin-2-yl)-2-aza-bicyclo[2.2.2]octan-3-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 2-Azabicyclo(2.2.2)octan-3-one | HCID 137887 | — |
| Edukt | 2-Chloro-6,7-dimethoxyquinoxaline | HCID 22573137 | — |
| Lösungsmittel | tetrahydrofuran N,N-dimethylformamide | HCID 21974620 | — |
| Produkt | 2-(6,7-Dimethoxy-quinoxalin-2-yl)-2-aza-bicyclo[2.2.2]octan-3-one | HCID 22573161 | 34,9% |
Reaktionsbedingungen
| Temperatur | 80 °C |
|---|
Reaktionsschritte
2-Azabicyclo[2.2.2]octan-3-one (228 mg. 2.3 mmole) is dissolved in a mixture of THF/DMF (5 mL/3 mL) and treated with NaH (60%, 184 mg, 4.6 mmole). The resulting mixture is heated at 60° C. for 0.5 hour before addition of 2-chloro-6,7-dimethoxyquinoxaline (344 mg, 1.5 mmole). After being heated at 80° C. overnight, the reaction mixture is concentrated. The residue is chromatographed on silica gel (50% ethyl acetate/hexane) to give 164 mg (23%) of a yellow solid (m.p. 158-159° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06696434B2 |
| Quelldatensatz | uspto-grants-2004_02 |
| ORD ID | ord-db5bc30d0a5247eeb29482d24063882d |
| Quellennotiz | uspto-grants-2004_02 |