Réaction #2317942

ord-a03b69f823da40f4af31a666749edcd8

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Concentrationconcentration
  2. 2
    Autreby evaporation
  3. 3
    Lavagethe organic phase is washed with sodium carbonate solution
  4. 4
    Séchagedried with sodium sulfate
  5. 5
    workup.ADDITIONThe filtrate is mixed with hexane
  6. 6
    Filtrationthe precipitate is filtered out
  7. 7
    Autredried

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06426059B1uspto-grants-2002_07