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Potassium Carbonate → 1,5-Dichloro-2-fluoro-3-(3,3,3-trifluoroprop-1-en-2-yl)benzene

HRID 2206927
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2206927
BrC1C=C(Cl)C=C(Cl)C=1F.FC(F)(F)C(B(O)O)=C.C(=O)([O-])[O-].[K+].[K+].[Cl:26][C:27]1[CH:32]=[C:31]([C:33]([C:35]([F:38])([F:37])[F:36])=[CH2:34])[C:30]([F:39])=[C:29]([Cl:40])[C:28]=1F>O1CCCC1.O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.CCCCCC>[Cl:40][C:29]1[CH:28]=[C:27]([Cl:26])[CH:32]=[C:31]([C:33]([C:35]([F:36])([F:37])[F:38])=[CH2:34])[C:30]=1[F:39]
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Komponenten

9

Edukt 4

HCID 11430Potassium CarbonateHCID 2782677(3,3,3-Trifluoroprop-1-en-2-yl)boronic acidHCID 509978971-Bromo-3,5-dichloro-2-fluorobenzeneHCID 866850801,3-Dichloro-2,4-difluoro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene

Produkt 1

HCID 871590141,5-Dichloro-2-fluoro-3-(3,3,3-trifluoroprop-1-en-2-yl)benzene

Reagenzien, Katalysatoren, Lösungsmittel

4
HCID 178418476HCID 178418476, VerbindungKatalysatorHCID 962WaterLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittelHCID 8058HexaneLösungsmittel2×

Versuchsvorschrift

1-bromo-3,5-dichloro-2-fluorobenzene (10 g), (3,3,3-trifluoroprop-1-en-2-yl)-boronic acid (7.5 g) and potassium carbonate (13.6 g) were dissolved in tetrahydrofuran (41 ml) and water (20 ml), and then deaerated. Dichlorobis(triphenylphosphine)palladium (II) (1.4 g) was added thereto and the mixture was stirred for 3 hours under reflux under argon atomosphere. After cooling the mixture to the room temperature, water and n-hexane were added, and the organic layer was washed with water and dried over anhydrous magnesium sulfate. The drying agent was filtered off, the solvent was distilled off under reduced pressure, and the residue was roughly purified by silica gel chromatography (n-hexane) to obtain a mixture containing 1,3-dichloro-2,4-difluoro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene and hexane.

Aufarbeitung

  1. temperatureunder reflux under argon atomosphere
  2. additionwere added
  3. washthe organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationThe drying agent was filtered off
  6. distillationthe solvent was distilled off under reduced pressure
  7. customthe residue was roughly purified by silica gel chromatography (n-hexane)
  8. customto obtain a mixture

Quellen und Nachweise

ORD-Eintrag
ord-371fd72d8e624aa7a9fb9e25e228fb37
Quelldatensatz
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09375000B2

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