Reaktion #640521

ord-77896f8fc5af43b394fa71834f395fe8

Reaktionsgleichung

Nc1nonc1-c1nc2ccccc2[nH]1
4-(1H-benzimidazol-2-yl)-furazan-3-ylamine
CO
methanol
C=CC#N
acrylonitrile
N#CCCNc1nonc1-c1nc2ccccc2[nH]1
title compound
N#CCCNc1nonc1-c1nc2ccccc2[nH]1
4-(1H-Benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeEvaporation of the solvent under reduced pressure
  2. 2
    Sonstigepartitioning of the resulting residue between water and ethyl acetate
  3. 3
    Trocknenby drying of the organic solution over sodium sulphate

Vorschrift

To a solution of 4-(1H-benzimidazol-2-yl)-furazan-3-ylamine (0.10 g, 0.497 mmol) in pyridine (5 ml) sodium in methanol (0.02 g, 0.86 mmol in 1 ml) and acrylonitrile (0.03 g, 0.39 mmol) are added sequentially at 0° C. The mixture is stirred over night. Evaporation of the solvent under reduced pressure and partitioning of the resulting residue between water and ethyl acetate followed by drying of the organic solution over sodium sulphate gives the title compound in pure form. 1H-NMR (400 MHz, d6-DMSO): 13.7 (s, 1H); 7.82 (d, 1H); 7.60 (d, 1H); 7.36 (m, 2H); 7.20 (t, 1H); 3.67 (q, 2H); 2.94 (t, 2H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: USRE042890E1uspto-grants-2011_11