반응 #1435687

ord-2d8d2fe7a11b4ea4b423f0de1f4b89f9

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축concentration
  2. 2
    기타by evaporation
  3. 3
    세척the organic phase is washed with sodium carbonate solution
  4. 4
    건조dried with sodium sulfate
  5. 5
    workup.ADDITIONThe filtrate is mixed with hexane
  6. 6
    여과the precipitate is filtered out
  7. 7
    기타dried

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07211241B2uspto-grants-2007_05