HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 1-(3,5-Bis(trifluoromethyl)benzoyl)piperidin-4-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 3,5-Bis(trifluoromethyl)benzoyl chloride | HCID 101856 | — |
| Edukt | 4-Piperidinone trifluoroacetate | HCID 22285601 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 1-(3,5-Bis(trifluoromethyl)benzoyl)piperidin-4-one | HCID 11209963 | 94,5% |
Reaktionsschritte
A solution of 3,5-bis-trifluoromethyl-benzoyl chloride (17.4 g, 63 mmol) in dichloromethane (30 mL) was added with cooling to a solution of 4-piperidone trifluoroacetate (13.4 g, 63 mmol) and triethylamine (22 mL, 158 mmol) so that the temperature did not rise above 20° C. Stirring continued for 2 h at room temperature. Water was added, the phases were separated and the water phase was extracted with dichloromethane. The organic phases were pooled, dried with MgSO4 and the solvent was evaporated. Chromatography on silica gel (ethyl acetate/n-hexane 1:1) yielded the desired product (20.2 g, 94%), m.p. 155-157° C. and MS: m/e=339.1 (M+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06482829B2 |
| Quelldatensatz | uspto-grants-2002_11 |
| ORD ID | ord-d7db36838d9644d9a7b6a80cabe8f8cc |
| Quellennotiz | uspto-grants-2002_11 |