Реакция #1379897

ord-40560b34d0344e9a881657df5ce95af3

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas heated
  2. 2
    Температураat reflux for 24 hours
  3. 3
    ДругоеThe excess reagent was removed under reduced pressure
  4. 4
    Другоеthe resulting oil was purified by flash chromatography
  5. 5
    workup.ADDITIONa mixture of dichloromethane and ethyl acetate (60:40)
  6. 6
    Промывкаto elute the desired material
  7. 7
    ДругоеFractions were collected

Методика

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).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07238339B2uspto-grants-2007_07