Reaktion #450453
ord-44d657dd93a14d4a9555e1b08402b1a6
Reaktionsgleichung
benzyl cyanoformate
diethylenetriamine
triethylamine
→
Bis[2-(benzyloxycarbonylamino)-ethyl]-amine
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Einengenconcentration
- 2Sonstigeby evaporation
- 3Waschenthe organic phase is washed with sodium carbonate solution
- 4Trocknendried with sodium sulfate
- 5workup.ADDITIONThe filtrate is mixed with hexane
- 6Filtrationthe precipitate is filtered out
- 7Sonstigedried
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.