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Phenol → HCID 22995028, Verbindung

HRID 1168040
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1168040
Cl[C:2]1([CH3:10])[CH2:7][CH2:6][C:5](Cl)([CH3:8])[CH2:4][CH2:3]1.[C:11]1([OH:17])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[Cl-].[Al+3].[Cl-].[Cl-]>>[CH3:10][C:2]12[CH2:7][CH2:6][C:5]([CH3:8])([CH2:4][CH2:3]1)[C:14]1[CH:15]=[CH:16][C:11]([OH:17])=[CH:12][C:13]2=1
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Komponenten

4

Edukt 3

HCID 996PhenolHCID 6451240Aluminum(III) ChlorideHCID 124109771,4-Dichloro-1,4-dimethylcyclohexane2×

Produkt 1

HCID 22995028HCID 22995028, Verbindung

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

To a solution of 1,4-dichloro-1,4-dimethylcyclohexane (Compound 1, 3 g, 16.5 mmol) and phenol (1.55 g, 16.5 mmol) under argon at 25° C. was slowly added aluminum chloride (0.22g, 0.165 mmol). The resulting mixture was heated to 120° C. for 12 hours, and then it was quenched with ice. The products were extracted with CH2Cl2, the layers separated, and the organic layer was washed with water and brine. The organic layer was dried over Na2SO4, and filtered, and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using ethyl acetate:hexane (1:9) to yield the title compound as a yellow oil.

Aufarbeitung

  1. customat 25° C.
  2. customit was quenched with ice
  3. extractionThe products were extracted with CH2Cl2
  4. customthe layers separated
  5. washthe organic layer was washed with water and brine
  6. dry with materialThe organic layer was dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by column chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-47af6a6381c545718f2f1353aee59f23
Quelldatensatz
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06620963B1

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