2-(4-Ethoxy-2,3-difluorophenyl)-5-vinylselenophene → HCID 59456284, Verbindung

HRID 1873398

Reaktionsgleichung

Reaktionsgleichung von HRID 1873398
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[Se:11][C:12]([CH:15]=[CH2:16])=[CH:13][CH:14]=2)=[C:6]([F:17])[C:5]=1[F:18])[CH3:2]>C(OCC)(=O)C.[Pd]>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[Se:11][C:12]([CH2:15][CH3:16])=[CH:13][CH:14]=2)=[C:6]([F:17])[C:5]=1[F:18])[CH3:2]

Komponenten

4

Edukt 1

HCID 594563452-(4-Ethoxy-2,3-difluorophenyl)-5-vinylselenophene

Produkt 1

HCID 59456284HCID 59456284, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

1.50 g (4.77 mmol) of 2-(4-ethoxy-2,3-difluorophenyl)-5-vinylselenophene are hydrogenated in 15 ml of ethyl acetate, in the presence of Pd/C (5% of Pd) at atmospheric pressure and RT. The reaction soln. is filtered and concentrated to dryness, and the crude product is purified by column chromatography (SiO2, n-heptane:EtOAc=5:1). The further purification is carried out by recrystallisation from n-heptane. 2-(4-Ethoxy-2,3-difluorophenyl)-5-ethylselenophene is obtained as a colourless solid (m.p. 52° C.).

Aufarbeitung

  1. filtrationis filtered
  2. concentrationconcentrated to dryness
  3. customthe crude product is purified by column chromatography (SiO2, n-heptane:EtOAc=5:1)
  4. customThe further purification
  5. customis carried out by recrystallisation from n-heptane

Quellen und Nachweise

ORD-Eintrag
ord-0c8e6fe3cf694f83a5c05e74222116a9
Quelldatensatz
uspto-grants-2012_11
Patentnummer
US08304036B2

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