反応 #640531

ord-57cb82a95d384ee4b75e6f8e4bb38f56

反応方程式

Nc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)c([N+](=O)[O-])c1
4-[1-(4-chloro-3-nitrophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine
Nc1cc(C(=O)Cn2c(-c3nonc3N)nc3ccccc32)ccc1Cl
title compound
Nc1cc(C(=O)Cn2c(-c3nonc3N)nc3ccccc32)ccc1Cl
4-[1-(3-Amino-4-chlorophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過Filtration and evaporation at reduced pressure
  2. 2
    その他gives the crude product
  3. 3
    その他Purification
  4. 4
    抽出by extraction with ethyl acetate and chromatography on silicagel

実験手順

To a stirred solution of 4-[1-(4-chloro-3-nitrophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine (0.07 g, 0.175 mmol) in ethanol (6 ml) and water (1 ml) is added two drops of concentrated hydrochloric acid and iron powder (0.1 g, 17.5 mmol). The reaction mixture is heated at 80° C. for 8 hours. Filtration and evaporation at reduced pressure gives the crude product. Purification by extraction with ethyl acetate and chromatography on silicagel yields the title compound as colorless solid, m.p. 228-230° C.

出典

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