Reaktion #40584

Reaktionsgleichung

5-amino-2-(trifluoromethyl)pyridine

iodine

→

solid

Ausbeute 96.0%

3-Amino-2-iodo-6-(trifluoromethyl)pyridine

Ausbeute 96.0%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solid in suspension in the medium is removed by filtration
2. 2
   Einengenthe filtrate is concentrated under reduced pressure
3. 3
   Waschenwashed with 5% sodium hydroxide solution
4. 4
   Trocknenwith water and dried over magnesium sulfate
5. 5
   SonstigeThe solution obtained
6. 6
   Einengenis concentrated under reduced pressure and 3.42 g of the expected compound

Vorschrift

3.85 g (12.3 mM) of silver sulfate are added, with stirring and at room temperature, to a solution of 2 g (12.3 mM) of 5-amino-2-(trifluoromethyl)pyridine in 100 ml of ethanol. 3.13 g of iodine are then added and the reaction mixture is stirred at room temperature for 24 hours. The solid in suspension in the medium is removed by filtration and the filtrate is concentrated under reduced pressure. The evaporation residue is taken up in 200 ml of dichloromethane and washed with 5% sodium hydroxide solution, and then with water and dried over magnesium sulfate. The solution obtained is concentrated under reduced pressure and 3.42 g of the expected compound are thus obtained in the form of a pink solid (yield=96%).

Quelle