Methane → HCID 66733858, Verbindung

HRID 1929616Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1929616
[CH2:1]([O:5][C:6](=[O:18])[CH:7]=[CH:8][C:9]1[CH:14]=[C:13]([F:15])[C:12]([CH3:16])=[C:11]([F:17])[CH:10]=1)[CH2:2][CH2:3][CH3:4].C>[Pd].CO>[CH2:1]([O:5][C:6](=[O:18])[CH2:7][CH2:8][C:9]1[CH:14]=[C:13]([F:15])[C:12]([CH3:16])=[C:11]([F:17])[CH:10]=1)[CH2:2][CH2:3][CH3:4]

Komponenten

5

Edukt 2

HCID 297MethaneHCID 66733998HCID 66733998, Verbindung

Produkt 1

HCID 66733858HCID 66733858, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 3-(3,5-difluoro-4-methyl-phenyl)-acrylic acid butyl ester (7.651 g; 30.089 mmol) and 10% palladium over activated charcoal (0.760 g) was placed under nitrogen before MeOH (100 ml) was carefully added. The resulting suspension was placed under vacuum, then under hydrogen (1 atm), and the reaction mixture was vigorously stirred at rt for 2 h45. The reaction mixture was filtered over a pad of celite, and concentrated under reduced pressure to give the expected product 3-(3,5-difluoro-4-methyl-phenyl)-propionic acid butyl ester as a yellow oil which was further dried under HV (6.960 g; 90%). LC-MS: tR=1.10 min; [M+H]+: no ionisation.

Aufarbeitung

  1. additionwas carefully added
  2. filtrationThe reaction mixture was filtered over a pad of celite
  3. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-f22a620250634a2eb9b20ad420dd3967
Quelldatensatz
uspto-grants-2012_05
Patentnummer
US08188082B2

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