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Diisopropyl Ether → 1,2-Dichloro-3-(trifluoromethyl)-5-[1-(trifluoromethyl)ethenyl]benzene

HRID 885823
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 885823
Br[C:2]1[CH:3]=[C:4]([Cl:13])[C:5]([Cl:12])=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.C(OC(C)C)(C)C.C([Li])CCC.COB(OC)OC.Br[C:34]([C:36]([F:39])([F:38])[F:37])=[CH2:35].C(=O)([O-])[O-].[K+].[K+]>CCCCCC.O1CCCC1.CC(C1C=CC=C(C(C)C)C=1N1C(=[Pd])N(C2C(C(C)C)=CC=CC=2C(C)C)C=C1)C.CC(C1C=CC=C(C(C)C)C=1N1C(=[Pd])N(C2C(C(C)C)=CC=CC=2C(C)C)C=C1)C.C1C=C2C(C(C=CC2=O)=O)=CC=1.C1C=C2C(C(C=CC2=O)=O)=CC=1.C(OCC)(=O)C.O>[Cl:13][C:4]1[CH:3]=[C:2]([C:34]([C:36]([F:39])([F:38])[F:37])=[CH2:35])[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[C:5]=1[Cl:12]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

12

Edukt 6

HCID 7914Diisopropyl EtherHCID 8470Trimethyl borateHCID 11430Potassium CarbonateHCID 2726961-Propene, 2-bromo-3,3,3-trifluoro-HCID 250672915-Bromo-1,2-dichloro-3-(trifluoromethyl)benzeneHCID 178418339Butyllithium

Produkt 1

HCID 86643384
1,2-Dichloro-3-(trifluoromethyl)-5-[1-(trifluoromethyl)ethenyl]benzene
Ausbeute 79,1 %

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 111824871,3-Bis(2,6-diisopropylphenyl)imidazol-2-ylidene(1,4-naphthoquinone)palladium(0) dimerKatalysatorHCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 8058HexaneLösungsmittel2×HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a stirred solution of 5-bromo-2,3-dichlorobenzotrifluoride (26.2 g) and diisopropyl ether (9.1 g) in hexane (250 mL) at −10° C. was added dropwise 1.55M n-butyllithium in hexane (57.5 mL). After stirring at same temperature for 0.5 hour, trimethoxyborane (9.26 g) in tetrahydrofuran (30 mL) was added dropwise. After a further 10 minutes, water (150 mL), 2-bromo-3,3,3-trifluoropropene (23.4 g), potassium carbonate (36.9 g) and 1,3-bis(2,6-diisopropylphenyl)imidazol-2-ylidene(1,4-naphthoquinone)palladium(0) dimer (0.131 g) were added to the reaction mixture, which was stirred at 60° C. for 4 hours. After the completion of the reaction, the reaction mixture was cooled to room temperature, poured into ice-water (50 mL) and ethyl acetate (75 mL) and filtered. The filtrate was separated, and the organic layer was washed with water and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to provide a residue. The residue was purified by column chromatography on silica gel eluted with hexane to afford the title compound as a colorless oil (21.8 g).

Aufarbeitung

  1. waitAfter a further 10 minutes
  2. stirringwas stirred at 60° C. for 4 hours
  3. customAfter the completion of the reaction
  4. filtrationfiltered
  5. customThe filtrate was separated
  6. washthe organic layer was washed with water and brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customto provide a residue
  10. customThe residue was purified by column chromatography on silica gel
  11. washeluted with hexane

Quellen und Nachweise

ORD-Eintrag
ord-908b124911474cbf91b3c2baae6d9605
Quelldatensatz
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08242283B2

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