Methanol → 1,3-Di-tert-butylbenzene

HRID 2061956Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2061956
CS(O[C:6]1[CH:11]=[CH:10][C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:8][C:7]=1[C:16]([CH3:19])([CH3:18])[CH3:17])(=O)=O.C([O-])=O.[Li+].CO>[Pd].[C].O>[C:12]([C:9]1[CH:10]=[CH:11][CH:6]=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:8]=1)([CH3:15])([CH3:14])[CH3:13]

Komponenten

6

Edukt 3

HCID 887MethanolHCID 23680280Lithium formateHCID 445427162,4-Di-tert-butylphenyl methanesulfonate

Produkt 1

HCID 1368101,3-Di-tert-butylbenzeneAusbeute 75,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysator2×HCID 962WaterLösungsmittel

Versuchsvorschrift

Using the thus-obtained, regenerated Pd/carbon (10 g), the same reaction as in Example II-1 was carried out in a nitrogen atmosphere under normal pressure at 25° C., in which, however, 2,4-di-tert-butylphenyl methanesulfonate (100 g, 0.35 mols), lithium formate (37 g, 0.70 mols) and methanol (600 g) were used. Water (20 mL) was added to the reaction liquid and Pd/carbon was collected through filtration, and heptane (100 g) was added to the filtrate. The organic layer obtained after extraction was concentrated under reduced pressure to give crude 1,3-di-tert-butylbenzene (50 g, yield 75% by mass).

Aufarbeitung

  1. customthe same reaction as in Example II-1
  2. customwas carried out in a nitrogen atmosphere under normal pressure at 25° C., in which
  3. filtrationwas collected through filtration, and heptane (100 g)
  4. additionwas added to the filtrate
  5. customThe organic layer obtained
  6. extractionafter extraction
  7. concentrationwas concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6c0860746d36495db6d05fdabf44a465
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08283508B2

Notizen zur Reaktion

Wird geladen…