Thionyl Chloride → 1,1'-(Chloromethylene)bis(4-fluorobenzene)

HRID 414482

Reaktionsgleichung

Reaktionsgleichung von HRID 414482
[F:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6](O)[C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.S(Cl)([Cl:19])=O>O>[F:1][C:2]1[CH:16]=[CH:15][C:5]([CH:6]([Cl:19])[C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1

Komponenten

4

Edukt 2

HCID 24386Thionyl ChlorideHCID 1230494,4'-Difluorobenzhydryl alcohol

Produkt 1

HCID 27237731,1'-(Chloromethylene)bis(4-fluorobenzene)Ausbeute 90,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 5.00 g (22.7 mmol) of 4,4'-difluorobenzhydrol was added 16.5 ml (227 mmol) of thionyl chloride in the atmosphere of argon, and the mixture was stirred at room temperature for 30 minutes. To the resulting mixture was added water followed by extraction with benzene. The organic layer was successively washed with saturated sodium hydrogen carbonate solution and water, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue thus obtained was subjected to column chromatography on silica gel. There was yielded 4.90 g (20.5 mmol) of 4,4'-difluorobenzhydryl chloride from the fraction eluted with benzene.

Aufarbeitung

  1. extractionfollowed by extraction with benzene
  2. washThe organic layer was successively washed with saturated sodium hydrogen carbonate solution and water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue thus obtained

Quellen und Nachweise

ORD-Eintrag
ord-3105e40af57f46429c343abecd5a1306
Quelldatensatz
uspto-grants-1988_12
Patentnummer
US04792553

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