HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Oxalic Acid → HCID 25143818, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Oxalic Acid | HCID 971 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | Chromate | HCID 24461 | — |
| Edukt | 2-Bromoethyl methyl ether | HCID 80972 | — |
| Edukt | 3-(2,3-Difluorophenyl)pyrrolidin-3-ol | HCID 63988383 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | HCID 25143818 | HCID 25143818 | — |
Reaktionsschritte
Preparation according to Example 51: Enantiomer E1 of 3-(2,3-difluorophenyl)-pyrrolidin-3-ol (0.15 g, 0.75 mmol), acetonitrile (6 mL), potassium carbonate (0.208 g, 1.5 mmol) and 1-bromo-2-methoxyethane (0.07 mL, 0.75 mmol). Flash chromate-graphy on silica gel (Ethyl acetate/methanol, 10:1). Yield: 0.07 g. [α]D=+22.5°; The amine was converted to the oxalic acid salt and recrystallized from ethanol/diethyl ether/diisopropyl ether; M.p. 149-150° C.; MS m/z (relative intensity, 70 eV) 257 (M+, 1), 212 (bp), 182 (65), 127 (22), 141 (16), 213 (12).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08188301B2 |
| Quelldatensatz | uspto-grants-2012_05 |
| ORD ID | ord-a7074d322e6b4e9a9318b904d0017655 |
| Quellennotiz | uspto-grants-2012_05 |