Hydrochloric Acid → 2-Allyl-3,6-difluorophenol

HRID 1384071

Reaktionsgleichung

Reaktionsgleichung von HRID 1384071
C([O:4][C:5]1[CH:10]=[C:9]([F:11])[CH:8]=[CH:7][C:6]=1[F:12])C=C.Cl.CN(C)[C:16]1[CH:21]=CC=C[CH:17]=1>>[CH2:21]([C:10]1[C:9]([F:11])=[CH:8][CH:7]=[C:6]([F:12])[C:5]=1[OH:4])[CH:16]=[CH2:17]

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 949N,N-DimethylanilineHCID 107496562,5-Difluorophenol allyl ether

Produkt 1

HCID 108448632-Allyl-3,6-difluorophenol

Reaktionsbedingungen

Temperatur
170 °C

Versuchsvorschrift

The 2,5-difluorophenol allyl ether (13 g) was dissolved in N,N-dimethylaniline (90 ml) and the resulting solution was stirred under a nitrogen gas stream at 170° C. for 5 hr. Then the liquid reaction mixture was poured into a 10% aqueous solution of hydrogen chloride and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (developing solvent: 7% ethyl acetate/n-hexane) to give 2-allyl-3,6-difluorophenol (7.8 g) as a colorless oil.

Aufarbeitung

  1. customThen the liquid reaction mixture
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by silica gel column chromatography (developing solvent: 7% ethyl acetate/n-hexane)

Quellen und Nachweise

ORD-Eintrag
ord-32e18329d084413c8c3d50c9c45f4cd1
Quelldatensatz
uspto-grants-2001_07
Patentnummer
US06258811B1

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