Iodine → 1,2-Bis(2-(trifluoromethyl)phenyl)disulfane

HRID 335212

Reaktionsgleichung

Reaktionsgleichung von HRID 335212
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[SH:9].II>C(#N)C>[F:11][C:2]([F:1])([F:10])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[S:9][S:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[C:2]([F:11])([F:10])[F:1]

Komponenten

4

Edukt 2

HCID 807IodineHCID 27778892-(Trifluoromethyl)benzenethiol

Produkt 1

HCID 113256811,2-Bis(2-(trifluoromethyl)phenyl)disulfaneAusbeute 88,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A solution of 2-(trifluoromethyl)benzenethiol (0.185 mL, 1.40 mmol) in wet acetonitrile (1:5 water/acetonitrile) was added Iodine (0.178 g, 0.702 mmol) and allowed to stir over night at room temperature. The reaction was concentrated, then diluted with EtOAc and quenched with aqueous sodium thiosulfate, extracted and dried organic with brine, Na2SO4, filtered and concentrated to afford the title compound (219 mg, 44% yield) as a colorless oil.

Aufarbeitung

  1. concentrationThe reaction was concentrated
  2. additiondiluted with EtOAc
  3. customquenched with aqueous sodium thiosulfate
  4. extractionextracted and dried organic with brine, Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-8686f30af43d42c38c3c3a12ee695cf5
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08883828B2

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