反应 #40584

反应方程式

5-amino-2-(trifluoromethyl)pyridine

iodine

→

solid

收率 96.0%

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

收率 96.0%

溶剂

ethanol

反应条件

后处理

1. 1
   其他The solid in suspension in the medium is removed by filtration
2. 2
   浓缩the filtrate is concentrated under reduced pressure
3. 3
   洗涤washed with 5% sodium hydroxide solution
4. 4
   干燥with water and dried over magnesium sulfate
5. 5
   其他The solution obtained
6. 6
   浓缩is concentrated under reduced pressure and 3.42 g of the expected compound

实验过程

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%).

来源