HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonium Acetate → HCID 54187452, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonium Acetate | HCID 517165 | — |
| Edukt | Sodium cyanoborohydride | HCID 5003444 | — |
| Edukt | (2R,5S)-5-Chloro-2-{2-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzaldehyde | HCID 53673807 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 54187452 | HCID 54187452 | 99,1% |
Reaktionsschritte
To a solution of (2R,5S)-5-chloro-2-{2-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzaldehyde (1.86 g, 4.44 mmol) in MeOH (20 mL) was added ammonium acetate (3.42 g, 44 mmol) and sodium cyanoborohydride (0.195 g, 3.1 mmol). The resulting mixture was stirred overnight at ambient temperature. The reaction was quenched with concentrated hydrochloric acid and concentrated in vacuo. The residue was dissolved in water and basified with aqueous 3N NaOH (pH>10). The product was extracted with dichloromethane (2×) and ethyl acetate (2×). The combined organics were dried over magnesium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel gave the title compound (1.29 g, 69% yield)
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06649611B2 |
| Quelldatensatz | uspto-grants-2003_11 |
| ORD ID | ord-c4ef7363554341ffa01d88267800552d |
| Quellennotiz | uspto-grants-2003_11 |