Diisopropylamine → 1-Bromo-3-chloro-2,4-difluorobenzene

HRID 1699997

Reaktionsgleichung

Reaktionsgleichung von HRID 1699997
C(NC(C)C)(C)C.[F:8][C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=1[Br:16].[Cl:17]C(Cl)(Cl)C(C(Cl)(Cl)Cl)=O>C([Li])CCC>[Cl:17][C:14]1[C:9]([F:8])=[C:10]([Br:16])[CH:11]=[CH:12][C:13]=1[F:15]

Komponenten

5

Edukt 3

HCID 7912DiisopropylamineHCID 8303HexachloroacetoneHCID 676741-Bromo-2,4-difluorobenzene

Produkt 1

HCID 27732561-Bromo-3-chloro-2,4-difluorobenzene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 178418339ButyllithiumLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of 19 ml (0.135 mole) of diisopropylarnine in 125 ml of tetrahydroflran (TBF) cooled at −20° C. is added 80 ml of n-butyllithium (1.6 M in hexane). The temperature is raised to 0° C. for 5 minutes and lowered to −78° C. Then 25 g (0.129 mole) of 2,4-difluoro-bromobenzene is then added and the reaction is stirred at −65° C. for 2 hours. Then, 25 ml (0.164 mole) of hexachloroacetone is added and the solution is warmed at room temperature. After evaporation of the solvent, the residue is distilled under vacuum to give the desired product.

Aufarbeitung

  1. customlowered to −78° C
  2. temperaturethe solution is warmed at room temperature
  3. customAfter evaporation of the solvent
  4. distillationthe residue is distilled under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-8c047c2ef56049ac90d663ea63b103bc
Quelldatensatz
uspto-grants-2002_02
Patentnummer
US06348624B1

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