反応 #1379897

ord-40560b34d0344e9a881657df5ce95af3

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    温度at reflux for 24 hours
  3. 3
    その他The excess reagent was removed under reduced pressure
  4. 4
    その他the resulting oil was purified by flash chromatography
  5. 5
    workup.ADDITIONa mixture of dichloromethane and ethyl acetate (60:40)
  6. 6
    洗浄to elute the desired material
  7. 7
    その他Fractions were collected

実験手順

A solution of 2-(2-aminoethylamino)ethanol (4.6648 g; 44.8 mmole) dissolved in 35 mL of benzyl acrylate was heated at reflux for 24 hours. The excess reagent was removed under reduced pressure and the resulting oil was purified by flash chromatography using a mixture of dichloromethane and ethyl acetate (60:40) to elute the desired material. Fractions were collected and analyzed to determine which of these contain the product. Solvents were eliminated under vacuum to give 5.8 g (21.9%) of N,N,N′-tris[2-(benzyloxycarbonylethyl]-2-(2aminoethylamino)ethanol (8).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07238339B2uspto-grants-2007_07