HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 1-(4-Fluorophenyl)-4-oxocyclohexanecarbonitrile
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Methyl 5-cyano-5-(4-fluorophenyl)-2-oxocyclohexanecarboxylate | HCID 12230235 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 1-(4-Fluorophenyl)-4-oxocyclohexanecarbonitrile | HCID 91805 | 62,9% |
Reaktionsschritte
101.5 g of 5-Cyano-5-(4-fluoro-phenyl)-2-oxo-cyclohexanecarboxylic acid methyl ester (11) were dissolved in 680 mL of ethanol and 171 mL of concentrated aqueous hydrochloric acid were added. The mixture was heated to reflux for 40 h, then evaporated. The residue was taken up in water and extracted with dichloromethane. The organic layer was washed with brine, dried over magnesium sulphate and evaporated to give 95.2 g of crude product, that was purified by silica gel filtration (heptanes:ethyl acetate) to yield 50.4 g of the desired product 12. Rt=1.26 min (Method 1). Detected mass: 218.2 (M+H+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08541449B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-73d1812c7d0141128be68c792624f4f6 |
| Quellennotiz | uspto-grants-2013_09 |