反応 #40584

ord-d8ab2f2da6704ce983b0aa772fa77a07

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07728002B2uspto-grants-2010_06