반응 #40584

반응 방정식

5-amino-2-(trifluoromethyl)pyridine

iodine

→

solid

수율 96.0%

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

수율 96.0%

용매

ethanol

반응 조건

후처리

1. 1
   기타The solid in suspension in the medium is removed by filtration
2. 2
   농축the filtrate is concentrated under reduced pressure
3. 3
   세척washed with 5% sodium hydroxide solution
4. 4
   건조with water and dried over magnesium sulfate
5. 5
   기타The solution obtained
6. 6
   농축is concentrated under reduced pressure and 3.42 g of the expected compound

실험 절차

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%).

출처