Water → HCID 22227324, Verbindung

HRID 2395807Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2395807
Br[C:2]([F:16])([F:15])[C:3](F)([F:13])[O:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[O:10])=[CH:7][CH:6]=1.O>[Zn].C(#N)C>[F:13][C:3]([O:4][C:5]1[CH:12]=[CH:11][C:8]([CH:9]=[O:10])=[CH:7][CH:6]=1)=[C:2]([F:16])[F:15]

Komponenten

5

Edukt 2

HCID 962WaterHCID 18990557HCID 18990557, Verbindung

Produkt 1

HCID 22227324HCID 22227324, VerbindungAusbeute 63,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23994ZincKatalysatorHCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
79 °C

Versuchsvorschrift

Acetonitrile (300 ml) and granular zinc (30.0 g) are combined in a 1 liter round bottomed flask and stirred at 75° C. under nitrogen as 4-(2-bromotetrafluoroethoxy)benzaldehyde (111.39 g, 0.37 mole) is added slowly by dropping addition funnel. The resulting mixture is stirred and heated at 79° C. for 12 hours. After filtration to remove zinc salts and unreacted zinc, the acetonitrile is removed under vacuum on a rotary evaporator. The resulting oily residue is flash distilled on a rotary evaporator under high vacuum (26.6 Pa) to provide 47.33 g (0.234 mole) of a water white oil in 63.3 percent yield.

Aufarbeitung

  1. additionis added slowly
  2. additionaddition funnel
  3. filtrationAfter filtration
  4. customto remove zinc salts and unreacted zinc
  5. customthe acetonitrile is removed under vacuum on a rotary evaporator
  6. distillationdistilled on a rotary evaporator under high vacuum (26.6 Pa)

Quellen und Nachweise

ORD-Eintrag
ord-cdefe62b020d4375861ab2730fd1eb2d
Quelldatensatz
uspto-grants-1996_02
Patentnummer
US05489623

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