반응 #1379897

ord-40560b34d0344e9a881657df5ce95af3

반응 방정식

NCCNCCO
2-(2-aminoethylamino)ethanol
C=CC(=O)OCc1ccccc1
benzyl acrylate
NCCNC(CO)CCC(=O)OCc1ccccc1
2-(benzyloxycarbonylethyl]-2-(2aminoethylamino)ethanol

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도at reflux for 24 hours
  3. 3
    기타The excess reagent was removed under reduced pressure
  4. 4
    기타the resulting oil was purified by flash chromatography
  5. 5
    workup.ADDITIONa mixture of dichloromethane and ethyl acetate (60:40)
  6. 6
    세척to elute the desired material
  7. 7
    기타Fractions were collected

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07238339B2uspto-grants-2007_07