Reaktion #2330464

ord-d978de2a7d2b49fdaef6fcbf3c5c3439

Reaktionsgleichung

FC(F)(F)c1nc(S)n[nH]1
5-Trifluoromethyl-1H-(1,2,4)-triazole-3-thiol
FC(F)(F)C(F)(F)C(F)(F)I
heptafluoro-1-iodopropane
CCN(CC)CC
triethylamine
FC(F)(F)c1nc(SC(F)(F)C(F)(F)C(F)(F)F)n[nH]1
3-heptafluoropropylsulfanyl-5-trifluoromethyl-1H-(1,2,4)-triazole
Ausbeute 17.6%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with water and saturated aqueous solution of sodium chloride
  2. 2
    TrocknenAfter drying the organic layer with magnesium sulfate
  3. 3
    workup.DISTILLATIONthe solvent was distilled off under the reduced pressure

Vorschrift

5-Trifluoromethyl-1H-(1,2,4)-triazole-3-thiol (11.0 g), heptafluoro-1-iodopropane (3.5 g) and triethylamine (0.90 g) were stirred in DMF (10 ml) at 90° C. for 24 hours. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate and washed with water and saturated aqueous solution of sodium chloride. After drying the organic layer with magnesium sulfate, the solvent was distilled off under the reduced pressure to obtain 3-heptafluoropropylsulfanyl-5-trifluoromethyl-1H-(1,2,4)-triazole (0.70 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07674807B2uspto-grants-2010_03