HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Anhydride → 1-Acetyl-4-benzoylpiperidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Anhydride | HCID 7918 | — |
| Edukt | 4-Benzoylpiperidine hydrochloride | HCID 2724437 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 1-Acetyl-4-benzoylpiperidine | HCID 2740714 | — |
Reaktionsschritte
A mixture of phenyl(piperidin-4-yl)methanone hydrochloride (743 mg, 3.29 mmol, Apollo Scientific) in DCM (13.2 mL) and TEA (1.10 mL, 7.90 mmol) was treated with Ac2O (0.373 mL, 3.95 mmol) dropwise over 1 min on an ice bath under argon, and the resulting translucent mixture was immediately removed from the ice bath and stirred at room temperature overnight. The reaction was then partitioned with 1 M HCl (1×8 mL) and 1 M NaOH (1×8 mL), and the organic layer was dried (Na2SO4), filtered, and concentrated to provide the title compound as a translucent beige oil that crystallized upon standing.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09309222B2 |
| Quelldatensatz | uspto-grants-2016_04 |
| ORD ID | ord-7e76c6bd2a5040c4997c089712112ea1 |
| Quellennotiz | uspto-grants-2016_04 |