Reaktion #62038

Reaktionsgleichung

thiophosgene

4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylamine

sodium bicarbonate

→

crude product

Ausbeute 97.4%

4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylisothiocyanate

Ausbeute 97.4%

Lösungsmittel

chloroform

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe bottom layer of the mixture was separated
2. 2
   Extraktionthe aqueous layer was extracted twice with CHCl3
3. 3
   WaschenThe combined organic solution was washed with water
4. 4
   Trocknendried over Mg2SO4
5. 5
   Sonstigeevaporated

Vorschrift

4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylamine (1.36 g, 5 mmol) was dissolved in 150 ml of chloroform and 100 ml of saturated aqueous sodium bicarbonate was added. To this biphasic mixture was added dropwise a solution of thiophosgene (0.39 ml, 5 mmol) in 30 ml of chloroform at room temperature with vigorous stirring. The mixture was stirred vigorously for 1 hour at room temperature. The bottom layer of the mixture was separated, and the aqueous layer was extracted twice with CHCl3. The combined organic solution was washed with water, dried over Mg2SO4 and evaporated to give 1.53 g (97.4%) of crude product used for next step without further purification.

Quelle