Trifluoromethanesulfonic acid → HCID 66760033, Verbindung

HRID 2063808Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2063808
[CH3:1][O:2][C:3]1[C:8]([CH3:9])=[CH:7][C:6]([CH3:10])=[CH:5][C:4]=1[OH:11].FC(F)(F)S(O)(=O)=O>CCCCCCC>[CH3:1][O:2][C:3]1[C:4]2[O:11][C:6]([CH3:10])([CH3:7])[CH2:5][C:5]=2[C:6]([CH3:10])=[CH:7][C:8]=1[CH3:9]

Komponenten

4

Edukt 2

HCID 62406Trifluoromethanesulfonic acidHCID 64514463,5-Xylenol, 2-methoxy-2×

Produkt 1

HCID 66760033HCID 66760033, VerbindungAusbeute 202,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8900HeptaneLösungsmittel

Reaktionsbedingungen

Temperatur
55 °C

Versuchsvorschrift

Further, by using 2-methoxy-3,5-dimethylphenol (7.60 g, 41.7 mmol), synthesis was also performed according to the following method. That is, to a solution of n-heptane (76 mL) containing 2-methoxy-3,5-dimethylphenol (7.60 g, 41.7 mmol) and isobutyl aldehyde (5.71 mL, 62.6 mmol), trifluoromethanesulfonic acid (1.85 mL, 20.9 mmol) was added dropwise, and the mixture was stirred at 55° C. for 2.5 hours. After cooled to room temperature, the reaction solution was washed with water and dried using anhydrous magnesium sulfate, and then the solvent was removed under reduced pressure. The obtained residue was purified by basic silica gel chromatography (hexane-ethyl acetate 100:0) and silica gel chromatography (hexane-ethyl acetate 100:0-95:5) to give 8.70 g of the title compound (yield 100%).

Aufarbeitung

  1. additionwas added dropwise
  2. temperatureAfter cooled to room temperature
  3. washthe reaction solution was washed with water
  4. customdried
  5. customthe solvent was removed under reduced pressure
  6. customThe obtained residue was purified by basic silica gel chromatography (hexane-ethyl acetate 100:0) and silica gel chromatography (hexane-ethyl acetate 100:0-95:5)

Quellen und Nachweise

ORD-Eintrag
ord-78a81315e514446cb533775db84479ca
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08288390B2

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