Reaktion #486549

ord-b8b16aaaca1e4eaeb10499e1d4ff9603

Reaktionsgleichung

N#CC(=O)OCc1ccccc1
benzyl cyanoformate
NCCNCCN
diethylenetriamine
CCN(CC)CC
triethylamine
O=C(NCCNCCNC(=O)OCc1ccccc1)OCc1ccccc1
Bis[2-(benzyloxycarbonylamino)-ethyl]-amine

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenconcentration
  2. 2
    Sonstigeby evaporation
  3. 3
    Waschenthe organic phase is washed with sodium carbonate solution
  4. 4
    Trocknendried with sodium sulfate
  5. 5
    workup.ADDITIONThe filtrate is mixed with hexane
  6. 6
    Filtrationthe precipitate is filtered out
  7. 7
    Sonstigedried

Vorschrift

51.5 g (500 mmol) of diethylenetriamine and 139 ml (1 mol) of triethylamine are dissolved in dichloromethane and mixed at -20° C. with 161 g of benzyl cyanoformate (Fluka) in dichloromethane and then stirred overnight at room temperature. After the reaction is completed, concentration by evaporation is performed during draw-off, the residue is taken up in diethyl ether, the organic phase is washed with sodium carbonate solution and dried with sodium sulfate. The filtrate is mixed with hexane, the precipitate is filtered out and dried.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05820849uspto-grants-1998_10