HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethanol → HCID 58120261, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethanol | HCID 702 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Benzene, 2,4-dichloro-1-fluoro- | HCID 123112 | — |
| Edukt | (S)-3-((R)-2-Ethoxy-1-hydroxyethyl)pyrrolidine-1-carboxylic Acid t-Butyl Ester | HCID 66858889 | — |
| Lösungsmittel | Hydrochloric Acid | HCID 313 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 58120261 | HCID 58120261 | — |
Reaktionsschritte
(S)-3-((R)-2-Ethoxy-1-hydroxyethyl)pyrrolidine-1-carboxylic acid t-butyl ester (25.0 mg, 96.4 mmol) was dissolved in DMF (200 μL). NaH (2776 μg, 115.7 mmol) was added and the mixture was stirred at room temperature for 15 minutes. 2,4-Dichloro-1-fluorobenzene (22.6 μL, 192.8 μmol) was added and the mixture was stirred at 70° C. for 3 hours. The mixture was concentrated then dissolved in 1.2M HCl in EtOH (1.0 mL, 1.2 mmol) and stirred overnight. The product was concentrated and purified by preparative HPLC (10-40%, 60 min, BDS) to yield the title compound as a mono-TFA salt oil (24.4 mg, 100% purity). MS m/z: [M+H]+ calcd for C14H19Cl2NO2, 304.08; found 304.0.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08273786B2 |
| Quelldatensatz | uspto-grants-2012_09 |
| ORD ID | ord-e70328b0129d4c18a986025936216f11 |
| Quellennotiz | uspto-grants-2012_09 |