p-Toluenesulfonic acid monohydrate → 1,1'-(Prop-1-ene-1,1-diyl)bis(4-fluorobenzene)

HRID 1282471Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1282471
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)(O)[CH2:9][CH3:10])=[CH:4][CH:3]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([C:12]2[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=2)=[CH:9][CH3:10])=[CH:6][CH:7]=1

Komponenten

4

Edukt 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 18424484HCID 18424484, Verbindung

Produkt 1

HCID 184244971,1'-(Prop-1-ene-1,1-diyl)bis(4-fluorobenzene)Ausbeute 92 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

Into a reactor were introduced 2.80 g (11.3 mmol) of the 1,1-bis(4-fluorophenyl)propanol, 60 mL of toluene, and 14 mg of p-toluenesulfonic acid monohydrate under a nitrogen atmosphere. Azeotropic dehydration was conducted for 1 hour with toluene refluxing. After being cooled, the reaction mixture was washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution, subsequently dried with anhydrous magnesium sulfate, and then concentrated under reduced pressure to obtain 2.39 g (92%) of the target compound as white crystals.

Aufarbeitung

  1. temperatureAfter being cooled
  2. washthe reaction mixture was washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution
  3. dry with materialsubsequently dried with anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-59803f55663c495981c236257284bf15
Quelldatensatz
uspto-grants-2002_09
Patentnummer
US06455720B1

Notizen zur Reaktion

Wird geladen…