Lawesson's reagent → 4,4,4-Trifluorobutanethioamide

HRID 570742Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 570742
[F:1][C:2]([F:9])([F:8])[CH2:3][CH2:4][C:5]([NH2:7])=O.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:19]2)=CC=1>C1(C)C=CC=CC=1>[F:1][C:2]([F:9])([F:8])[CH2:3][CH2:4][C:5](=[S:19])[NH2:7]

Komponenten

4

Edukt 2

HCID 87949Lawesson's reagentHCID 12725184,4,4-Trifluorobutanamide

Produkt 1

HCID 537527964,4,4-TrifluorobutanethioamideAusbeute 73,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 4,4,4-trifluorobutanamide (17.9 g), 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide (51.3 g) and toluene (400 mL) was stirred at 80° C. for 3 hr. The reaction mixture was purified by aminopropylsilane-bonded silica gel column chromatography (ethyl acetate), and again purified by aminopropylsilane-bonded silica gel column chromatography (ethyl acetate/hexane) to give the title compound (14.6 g) as a solid.

Aufarbeitung

  1. customThe reaction mixture was purified by aminopropylsilane-
  2. customagain purified by aminopropylsilane-

Quellen und Nachweise

ORD-Eintrag
ord-817a1fb486f046d49147f73a70abb3d0
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09023858B2

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