反応 #76803

ord-94349ec1c95c4d0393ddc99632c72773

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to reflux under a nitrogen atmosphere
  2. 2
    その他the solvent was removed in vacuo
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in 20 mL of saturated aqueous sodium carbonate
  4. 4
    抽出extracted with chloroform (3×25 mL)
  5. 5
    抽出The combined organic extract
  6. 6
    乾燥was dried over anhydrous magnesium sulfate
  7. 7
    濃縮concentrated in vacuo

実験手順

A solution of 74 mg (0.295 mmol) of 4′-chlorospiro[1-azabicyclo[2.2.2]octane-3,2′(3′H)-furo[2,3-b]pyridine] in 10 mL of ethylenediamine was heated to reflux under a nitrogen atmosphere and stirred for 4 days. Upon cooling to ambient temperature, the solvent was removed in vacuo. The residue was dissolved in 20 mL of saturated aqueous sodium carbonate and extracted with chloroform (3×25 mL). The combined organic extract was dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title compound as a dark oil, 80 mg (100%): electrospray MS (m/z, relative intensity) 275 ([MH]+).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06703502B2uspto-grants-2004_03