Chlorotrimethylsilane → 1,2-Difluoro-3-trimethylsilylbenzene

HRID 257685

Reaktionsgleichung

Reaktionsgleichung von HRID 257685
C([Li])CCC.[F:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[F:13].[CH3:14][Si:15]([CH3:18])([CH3:17])Cl.C1COCC1>CCCCCC.O>[F:6][C:7]1[C:8]([F:13])=[CH:9][CH:10]=[CH:11][C:12]=1[Si:15]([CH3:18])([CH3:17])[CH3:14]

Komponenten

7

Edukt 4

HCID 6397ChlorotrimethylsilaneHCID 8028TetrahydrofuranHCID 97061,2-DifluorobenzeneHCID 178418339Butyllithium

Produkt 1

HCID 108993711,2-Difluoro-3-trimethylsilylbenzene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8058HexaneLösungsmittel

Versuchsvorschrift

12.5 ml of a 1.6-molar solution of n-butyllithium in hexane is added dropwise at 0° C. to a mixture of 0.02 mol of 1,2-difluorobenzene, 0.02 mol of trimethylchlorosilane and 25 ml of THF. After stirring at room temperature for 1.5 hours, the reaction mixture is poured into water, the phases are separated, and the aqueous phase is extracted with 2×50 ml of methylene chloride. Drying over magnesium sulfate, evaporation of the solvent and chromatography give the pure product.

Aufarbeitung

  1. customthe phases are separated
  2. extractionthe aqueous phase is extracted with 2×50 ml of methylene chloride
  3. dry with materialDrying over magnesium sulfate, evaporation of the solvent and chromatography
  4. customgive the pure product

Quellen und Nachweise

ORD-Eintrag
ord-8afda83419114c30a43bb1c65f1f85f2
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05262556

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