HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium hydride → HCID 178486824, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 2-Chloro-6,7-dimethoxyquinoxaline | HCID 22573137 | — |
| Edukt | HCID 178525780 | HCID 178525780 | — |
| Lösungsmittel | tetrahydrofuran N,N-dimethylformamide | HCID 21974620 | — |
| Produkt | HCID 178486824 | HCID 178486824 | — |
Reaktionsschritte
A mixture of cis/trans-4-hydroxy-cyclohexanecarboxylic acid (144 mg, 1 mmol) and NaH (60%, 160 mg, 4 mmol) in anhydrous THF/DMF (10 mL/2 mL) is refluxed for one hour before addition of 2-chloro-6,7-dimethoxyquinoxaline (225 mg, 1 mmol). The resulting mixture is continued to refluxed for four hours. The reaction mixture is neutralized to pH 5 and extracted with ethyl acetate (2×50 mL). The combined organic solutions are dried over magnesium sulfate and filtered. The residue after concentration is chromatographed on silica gel (ethyl acetate, followed by methanol) to provide the desired product as a white solid (m.p. 90-93° C.). Anal. Calcd. for C17H20N2O5.0.5 H2O: C, 59.89; H, 6.19; N, 8.22; Found: C, 59.91; H, 6.62; N, 7.90.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06852712B2 |
| Quelldatensatz | uspto-grants-2005_02 |
| ORD ID | ord-5f89f2b6a2b94f7fb98289f8b318ad40 |
| Quellennotiz | uspto-grants-2005_02 |