Reaktion #324183

Reaktionsgleichung

4-(4-chlorophenyl)-5-(2-thienyl)-1H-2-imidazolethiol

water

tetrafluoroethylene

→

4-(4-Chlorophenyl)-2-(1,1,2,2-tetrafluoroethylthio)-5-(2-thienyl)-1H-imidazole

Lösungsmittel

dimethylformamide

diisopropylamine

1-chlorobutane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe solution extracted with chloroform
2. 2
   SonstigeThe extract was dried
3. 3
   Einengenconcentrated
4. 4
   SonstigeIt was chromatographed on silica gel (Silicar CC-4)
5. 5
   Sonstigeto give 5.5 g of a cut which
6. 6
   Sonstigewas obtained

Vorschrift

A solution of 6.9 g of 4-(4-chlorophenyl)-5-(2-thienyl)-1H-2-imidazolethiol in 40 ml of dimethylformamide and 1.5 ml of diisopropylamine was pressured in a bomb with 3 g of tetrafluoroethylene and shaken until there was no further pressure drop. The bomb contents were poured into water, the pH adjusted to 8 and the solution extracted with chloroform. The extract was dried and concentrated. It was chromatographed on silica gel (Silicar CC-4) to give 5.5 g of a cut which was dissolved in hot 1-chlorobutane. On cooling 4.5 g of product was obtained, m.p. 161.5°-163° C.

Quelle