Azobisisobutyronitrile → 4-Acetylthio-1,1-bis(trifluoromethyl)-1-butanol

HRID 2218569

Reaktionsgleichung

Reaktionsgleichung von HRID 2218569
[F:1][C:2]([F:13])([F:12])[C:3]([C:8]([F:11])([F:10])[F:9])([OH:7])[CH2:4][CH:5]=[CH2:6].[C:14]([OH:17])(=[S:16])[CH3:15].CC(N=NC(C#N)(C)C)(C#N)C>N(C(C)(C)C#N)=NC(C)(C)C#N.O1CCOCC1>[C:14]([S:16][CH2:6][CH2:5][CH2:4][C:3]([C:8]([F:9])([F:10])[F:11])([C:2]([F:12])([F:13])[F:1])[OH:7])(=[O:17])[CH3:15]

Komponenten

6

Edukt 3

HCID 6547Azobisisobutyronitrile2×HCID 3288704-Penten-2-ol, 1,1,1-trifluoro-2-(trifluoromethyl)-HCID 178418634HCID 178418634, Verbindung2×

Produkt 1

HCID 865942984-Acetylthio-1,1-bis(trifluoromethyl)-1-butanolAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6547AzobisisobutyronitrileKatalysatorHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Under a nitrogen atmosphere, 20 g of 4,4-bis(trifluoromethyl)-4-hydroxy-1-butene (96.1 mmol), 8.05 g of thioacetic acid (105.7 mmol), 60 g of 1,4-dioxane and 0.79 g of 2,2′-azobisisobutyronitrile (hereinafter abbreviated as AIBN) (4.8 mmol) were put into a flask equipped with a stirring bar, a thermometer and a condenser, and heated with stirring. During the reaction, thioacetic acid and AIBN were appropriately added and after confirming that a substrate was completely consumed, the reaction solution was distilled as it was under reduced pressure to yield an intermediate product, 22 g of 4-acetylthio-1,1-bis(trifluoromethyl)-1-butanol (76.9 mmol).

Aufarbeitung

  1. customwere put into a flask
  2. customequipped with a stirring bar
  3. temperaturea thermometer and a condenser, and heated
  4. additionwere appropriately added
  5. customwas completely consumed
  6. distillationthe reaction solution was distilled as it

Quellen und Nachweise

ORD-Eintrag
ord-eb970c3d5fb043828d0f48b16c0cc4b5
Quelldatensatz
uspto-grants-2008_08
Patentnummer
US07411097B2

Verknüpfte Notizen

Wird geladen…