反応 #324183

反応方程式

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

溶媒

dimethylformamide

diisopropylamine

1-chlorobutane

反応条件

後処理

1. 1
   抽出the solution extracted with chloroform
2. 2
   その他The extract was dried
3. 3
   濃縮concentrated
4. 4
   その他It was chromatographed on silica gel (Silicar CC-4)
5. 5
   その他to give 5.5 g of a cut which
6. 6
   その他was obtained

実験手順

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.

出典