HCID 178471409, Verbindung → HCID 178471410, Verbindung

HRID 726507Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 726507
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C@H:9]1[CH2:14][CH2:13][C@H:12]([CH:15]=[CH:16][CH2:17][CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:11][CH2:10]1>C(OCC)(=O)C>[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C@H:9]1[CH2:10][CH2:11][C@H:12]([CH2:15][CH2:16][CH2:17][CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:13][CH2:14]1

Komponenten

3

Edukt 1

HCID 178471409HCID 178471409, Verbindung

Produkt 1

HCID 178471410HCID 178471410, VerbindungAusbeute 85,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

First, 9 g of 2,3-difluoro-1-[trans-4-(4-ethoxycarbonyl-1-butenyl)cyclohexyl]benzene, 0.5 g of 10% Pd--C, and 50 ml of ethyl acetate were placed in a 300 ml autoclave. The mixture was stirred for 3 days under a hydrogen pressure of 30 kg/cm2. A catalyst was filtered away and a filtrate was concentrated. Thereafter, the residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/1) to obtain 7.71 g of 2,3-difluoro-1-[trans-4-(4-ethoxycarbonylbutyl)cyclohexyl]benzene (Y: 85.1%). The compound thus obtained had a purity of 85% by GC.

Aufarbeitung

  1. filtrationA catalyst was filtered away
  2. concentrationa filtrate was concentrated
  3. customThereafter, the residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/1)

Quellen und Nachweise

ORD-Eintrag
ord-3df198bf693d4a6aa9d63b7adb65b1ed
Quelldatensatz
uspto-grants-1998_01
Patentnummer
US05709911

Notizen zur Reaktion

Wird geladen…