Reaktion #1379897

ord-40560b34d0344e9a881657df5ce95af3

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux for 24 hours
  3. 3
    SonstigeThe excess reagent was removed under reduced pressure
  4. 4
    Sonstigethe resulting oil was purified by flash chromatography
  5. 5
    workup.ADDITIONa mixture of dichloromethane and ethyl acetate (60:40)
  6. 6
    Waschento elute the desired material
  7. 7
    SonstigeFractions were collected

Vorschrift

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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07238339B2uspto-grants-2007_07