反応 #1106876

ord-dab2bd828e60411a9ec5e24385c50ac9

反応条件

温度
130°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool to room temperature
  2. 2
    その他The aqueous phase is separated out
  3. 3
    抽出extracted twice with chloroform
  4. 4
    洗浄the combined organic phases are washed with saturated aqueous sodium chloride solution
  5. 5
    乾燥dried over sodium sulfate
  6. 6
    濃縮the filtrate is concentrated under reduced pressure

実験手順

10.37 g (43.80 mmol) of 2,5-dibromopyridine, 10.00 g (43.80 mmol) of tert-butyl 2-piperidin-4-ylethylcarbamate and 6.05 g (43.80 mmol) of potassium carbonate are placed in an autoclave. The mixture is then heated at 130° C. for 12 hours. The reaction mixture is allowed to cool to room temperature and then taken up in chloroform and saturated aqueous sodium hydrogen carbonate solution. The aqueous phase is separated out and extracted twice with chloroform, and the combined organic phases are washed with saturated aqueous sodium chloride solution and dried over sodium sulfate, and the filtrate is concentrated under reduced pressure.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08716289B2uspto-grants-2014_05