HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 1-(4-Chlorophenyl)-4,4,4-trifluorobutane-1,3-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | P-Chloroacetophenone | HCID 7467 | — |
| Edukt | Ethyl trifluoroacetate | HCID 9794 | — |
| Edukt | Sodium Methoxide | HCID 10942334 | — |
| Lösungsmittel | tert-Butyl methyl ether | HCID 15413 | — |
| Produkt | 1-(4-Chlorophenyl)-4,4,4-trifluorobutane-1,3-dione | HCID 2773832 | 93,3% |
Reaktionsschritte
Ethyl trifluoroacetate (23.52 g, 166 mmol) was dissolved in methyl tert-butyl ether (75 mL). To the stirred solution was added 25 weight % sodium methoxide (40 mL, 177 mmol). Next 4'-chloroacetophenone (23.21 g, 150 mmol) was dissolved in methyl tert-butyl ether (20 mL), and added to the reaction dropwise. After stirring overnight (15.75 hours), 3N HCl (70 mL) was added. The organic layer was collected, washed with brine (75 mL), dried over MgSO4, filtered, and concentrated in vacuo to give a 35.09 g of yellow-orange solid. The solid was recrystallized from isooctane to give 31.96 g (85%) of the dione: mp 66-67° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06136839 |
| Quelldatensatz | uspto-grants-2000_10 |
| ORD ID | ord-e693ed903b2b4ba6bc55ef4c43944b5a |
| Quellennotiz | uspto-grants-2000_10 |