反応 #2069957

ord-0f3df3919ae94f048dc7b5f4ca7c0d04

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux for 1 hour 30 minutes
  2. 2
    温度The mixture was cooled on ice
  3. 3
    抽出extracted with ethyl acetate
  4. 4
    乾燥dried over anhydrous magnesium sulfate
  5. 5
    濃縮concentrated under reduced pressure
  6. 6
    その他The residue was purified by silica gel column chromatography

実験手順

Phosphorus oxychloride (1.6 ml) was added to a solution of the compound of Example B145 (600 mg, 1.7 mmol) in acetonitrile (15 ml), and the mixture was stirred under reflux for 1 hour 30 minutes. The mixture was cooled on ice, made alkaline with a 5% aqueous sodium hydrogencarbonate solution, extracted with ethyl acetate, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (82 mg).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07541332B2uspto-grants-2009_06