Реакция #640519

ord-3cfb0239468e46a7bb75299117b37dfd

Уравнение реакции

Nc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)cc1
4-[1-(4-chlorophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine
c1ccncc1
pyridine
CC(=O)Cl
acetyl chloride
CC(=O)Nc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)cc1
title compound
CC(=O)Nc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)cc1
N-{4-[1-(4-Chlorophenacyl)-1H-benzimidazol-2-yl]-furazan-3-yl}-acetamide

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Промывкаwashed with water
  2. 2
    Сушкаdried over sodium sulphate
  3. 3
    ФильтрацияFiltration of the sodium sulphate, concentration of the filtrate under reduced pressure and chromatography of the residue on silicagel

Методика

A solution of 4-[1-(4-chlorophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine (0.05 g, 0.143 mmol), pyridine (0.022 g, 0.282 mmol), acetyl chloride (0.013 g, 0.169 mmol) and a catalytic amount of DMAP in DMF (5 ml) is stirred at 80° C. for 16 hours. The reaction mixture is diluted with ethyl acetate, washed with water and dried over sodium sulphate. Filtration of the sodium sulphate, concentration of the filtrate under reduced pressure and chromatography of the residue on silicagel using hexane-ethyl acetate as eluent gives the title compound as a yellowish solid, m.p. 202-205° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: USRE042890E1uspto-grants-2011_11