HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl Acetate → 4-(4-Chlorophenyl)-3-cyano-3-phenyl-2-butanone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | Alpha-phenylacetoacetonitrile | HCID 20547 | — |
| Edukt | 1-(Bromomethyl)-4-chlorobenzene | HCID 69329 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 4-(4-Chlorophenyl)-3-cyano-3-phenyl-2-butanone | HCID 66430925 | — |
Reaktionsschritte
To a solution of α-acetylphenylacetonitrile (1.0 g, 6.3 mmol) in acetonitrile (25 mL) was added 4-chlorobenzyl bromide (1.3 g, 6.3 mmol) and cesium carbonate (8.2 g, 25 mmol). After stirring at room temperature for 2 h, the reaction mixture was poured into ethyl acetate (100 mL) and water (100 mL). The organic layer was separated, washed with brine, dried over magnesium sulfate, filtered, and concentrated to dryness, and the residue was purified on a silica gel column eluting with 1 to 5% ethyl acetate in hexane to give the title compound. 1H NMR (400 MHz, CD3OD): δ 7.5-6.9 (m, 9H), 3.56 (d, 1H), 3.37 (d, 1H), 2.22 (s, 3H). LC-MS: m/e 306 (M+Na)+ (3.0 min).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07423067B2 |
| Quelldatensatz | uspto-grants-2008_09 |
| ORD ID | ord-85f207f8293a41209effb383b5d70d18 |
| Quellennotiz | uspto-grants-2008_09 |