Реакция #640530

ord-5b55b11db96547dc8fe5cd334595eae2

Уравнение реакции

CC(=O)Nc1ccc(C(=O)Cn2c(-c3nonc3NCCC#N)nc3ccccc32)cc1
4-[1-(4-acetaminophenacyl)-1H-benzimidazol-2-yl]-furazan-3-yl-N-(2-cyanoethyl)-amine
O=C([O-])O.[Na+]
sodium bicarbonate
Nc1ccc(C(=O)Cn2c(-c3nonc3NCCC(=O)O)nc3ccccc32)cc1
title compound
Nc1ccc(C(=O)Cn2c(-c3nonc3NCCC(=O)O)nc3ccccc32)cc1
4-[1-(4-Aminophenacyl)-1H-benzimidazol-2-yl]-furazan-3-yl-N-(2-carboxyethyl)-amine

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураat reflux for two hours
  2. 2
    ЭкстракцияExtraction with ethyl acetate
  3. 3
    Сушкаdrying over sodium sulphate
  4. 4
    Фильтрацияfiltering
  5. 5
    Другоеevaporation of the resulting filtrate to dryness

Методика

A solution of 4-[1-(4-acetaminophenacyl)-1H-benzimidazol-2-yl]-furazan-3-yl-N-(2-cyanoethyl)-amine (0.061 g) in aqueous hydrochloric acid (5 ml, HCl conc.) is heated at reflux for two hours. The mixture is diluted with water and neutralized by addition of sodium bicarbonate. Extraction with ethyl acetate, drying over sodium sulphate, filtering and evaporation of the resulting filtrate to dryness gives the title compound in pure form, m.p. 174-177° C. 1H-NMR (400 MHz, d6-DMSO): 12.40 (s, 1H); 7.84 (m, 4H); 7.38 (m, 3H); 6.65 (m, 2H); 6.28 (S, 2H); 6.17 (s, 2H); 3.57 (m, 2H); 2.66 (t, 2H).

Источник

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