1,2,4-Trichlorobenzene → HCID 22737355, Verbindung

HRID 51084Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 51084
[F:1][C:2]([F:16])([F:15])[CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([O:11]CC=C)=[CH:7][CH:6]=1.Cl[C:18]1[CH:23]=CC(Cl)=C[C:19]=1Cl>>[CH2:23]([C:7]1[CH:6]=[C:5]([O:4][CH2:3][C:2]([F:1])([F:15])[F:16])[CH:10]=[CH:9][C:8]=1[OH:11])[CH:18]=[CH2:19]

Komponenten

3

Edukt 2

HCID 131,2,4-TrichlorobenzeneHCID 22737359Allyl 4-(2,2,2-trifluoroethoxy)phenyl ether

Produkt 1

HCID 22737355HCID 22737355, Verbindung

Versuchsvorschrift

A solution of allyl 4-(2,2,2-trifluoroethoxy)phenyl ether (1.9 g, 8.2 mmol) in 1,2,4-trichlorobenzene 30 ml was heated to 180° C. for 24 hr. The solvent was removed under reduced pressure, and the crude product was chromatographed on silica gel eluting with 20% AcOEt/hexanes to give 0.9 g of 2-allyl-4-(2,2,2-trifluoroethoxy)phenol. This material was dissolved in 30 ml ethanol and was hydrogenated with 15 mg of 10% Pd/C in a Parr shaker under hydrogen atmosphere (50 psi) overnight. The catalyst was removed by suction-filtration through a pad of celite. The filtrate was concentrated to give the title compound 0.73 g as a clear oil.

Aufarbeitung

  1. customThe solvent was removed under reduced pressure
  2. customthe crude product was chromatographed on silica gel eluting with 20% AcOEt/hexanes

Quellen und Nachweise

ORD-Eintrag
ord-494428eb1f00406aa5c166ef8373000c
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06713508B2

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