Reaktion #1784135

ord-54274d3c1c6e4dd8a3b2e584862bc5bf

Reaktionsgleichung

CC#N
acetonitrile
Nc1ccc(S)cc1
4-aminothiophenol
CCN(CC)CC
triethylamine
FC(F)(F)C(F)(F)C(F)(F)I
1-iodoheptafluoro-n-propane
Nc1ccc(SC(F)(F)C(F)(F)C(F)(F)F)cc1
desired product
Ausbeute 63.2%
Nc1ccc(SC(F)(F)C(F)(F)C(F)(F)F)cc1
4-(heptafluoro-n-propylthio) aniline
Ausbeute 63.2%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with aqueous 1N sodium hydroxide solution
  2. 2
    Sonstigepurified by silica gel column chromatography

Vorschrift

To 20 ml of an acetonitrile solution of 1.25 g of 4-aminothiophenol and 1.11 g of triethylamine was added 5.91 g of 1-iodoheptafluoro-n-propane. The resulting mixture was stirred at room temperature for 3 hours, diluted with ether, and then washed with aqueous 1N sodium hydroxide solution, purified by silica gel column chromatography using an eluent (development solvent; hexane:ethyl acetate=4:1) to obtain 1.85 g of the desired product (Yield: 63%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08163804B2uspto-grants-2012_04