2,6-Difluorobenzamide → 2,6-Difluorobenzene-1-carbothioamide

HRID 73597

Reaktionsgleichung

Reaktionsgleichung von HRID 73597
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4]([NH2:6])=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:21])=CC=1>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4](=[S:21])[NH2:6]

Komponenten

4

Edukt 2

HCID 874392,6-DifluorobenzamideHCID 87949Lawesson's reagent

Produkt 1

HCID 126832122,6-Difluorobenzene-1-carbothioamideAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

A solution of 2, 6 difluorobenzamide (1 eq) and Lawesson's reagent (0.5 eq.) in toluene (0.2 M) was heated at 90° C. for 14 hours. Upon cooling the volatiles were removed in vacuo and purified by SiO2 chromatography (25% EtOAc/hexanes) yielding 2,6-difluorobenzothioamide as a light yellow solid (99%). LCMS (m/z): 174.1 (MH+); LC Rt=2.19 min.

Aufarbeitung

  1. temperatureUpon cooling the volatiles
  2. customwere removed in vacuo
  3. custompurified by SiO2 chromatography (25% EtOAc/hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-b0b6e2c6e1cd425cb1c695a43492eb1a
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08829193B2

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