Reaktionsgleichung
Br[C:2]([F:6])=[C:3]([F:5])[F:4].Cl[Si:8]([CH3:19])([CH3:18])[C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH3:17])=[CH:11][CH:10]=1.C([Li])(CC)C.C1CCCCC1.Cl>CCOCC>[F:6][C:2]([Si:8]([CH3:18])([CH3:19])[C:9]1[CH:10]=[CH:11][C:12]([O:15][CH2:16][CH3:17])=[CH:13][CH:14]=1)=[C:3]([F:5])[F:4]Komponenten
7
Edukt 5
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- -65 °C
Versuchsvorschrift
A -30° C. solution of bromotrifluoroethylene (7.15 g, 0.044 mol) in ether is treated with p-(chlorodimethylsilyl)phenetole (9.54 g, 0.044 mol), cooled to -65° C., treated dropwise with a 1.3M solution of sec-butyllithium in cyclohexane (34.2 mL, 0.044 mol) while maintaining the temperature below -60° C., stirred at -65° C. for 5 hours, stirred at room temperature overnight, cooled to 0° C., treated with dilute hydrochloric acid, and diluted with ether. The organic phase is separated, washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a residue which is distilled to give the title product as a clear liquid (7.66 g, bp 84°-92° C./0.8 mm Hg).
Aufarbeitung
- temperaturewhile maintaining the temperature below -60° C.
- stirringstirred at room temperature overnight
- temperaturecooled to 0° C.
- customThe organic phase is separated
- washwashed with brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo
- customto obtain a residue which
- distillationis distilled
Quellen und Nachweise
- ORD-Eintrag
- ord-3bc9fb260f91463c93e8c4ad1090e966
- Quelldatensatz
- uspto-grants-1998_01
- Patentnummer
- US05710102
Verknüpfte Notizen
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