反应 #640530

ord-5b55b11db96547dc8fe5cd334595eae2

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度at reflux for two hours
  2. 2
    萃取Extraction with ethyl acetate
  3. 3
    干燥drying over sodium sulphate
  4. 4
    过滤filtering
  5. 5
    其他evaporation of the resulting filtrate to dryness

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE042890E1uspto-grants-2011_11