تفاعل #1379897

ord-40560b34d0344e9a881657df5ce95af3

معادلة التفاعل

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

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةat reflux for 24 hours
  3. 3
    أخرىThe excess reagent was removed under reduced pressure
  4. 4
    أخرىthe resulting oil was purified by flash chromatography
  5. 5
    workup.ADDITIONa mixture of dichloromethane and ethyl acetate (60:40)
  6. 6
    غسيلto elute the desired material
  7. 7
    أخرىFractions were collected

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07238339B2uspto-grants-2007_07