Реакция #1435687

ord-2d8d2fe7a11b4ea4b423f0de1f4b89f9

Уравнение реакции

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

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Концентрированиеconcentration
  2. 2
    Другоеby evaporation
  3. 3
    Промывкаthe organic phase is washed with sodium carbonate solution
  4. 4
    Сушкаdried with sodium sulfate
  5. 5
    workup.ADDITIONThe filtrate is mixed with hexane
  6. 6
    Фильтрацияthe precipitate is filtered out
  7. 7
    Другоеdried

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07211241B2uspto-grants-2007_05