反应 #640532

ord-bc19d117a55c4630b18be9f3c39e2601

反应方程式

Nc1nonc1-c1nc2ccccc2[nH]1
4-(1H-benzimidazol-2-yl)-furazan-3-ylamine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=C(CBr)c1ccc(Cl)c([N+](=O)[O-])c1
4-chloro-3-nitrophenacyl bromide
Nc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)c([N+](=O)[O-])c1
title compound
Nc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)c([N+](=O)[O-])c1
4-[1-(4-Chloro-3-nitrophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed with water
  2. 2
    干燥dried over sodium sulphate
  3. 3
    过滤Filtration of the sodium sulphate, concentration of the filtrate under reduced pressure and chromatography of the residue on silicagel

实验过程

A suspension of 4-(1H-benzimidazol-2-yl)-furazan-3-ylamine (0.228 g, 1.14 mmol), potassium carbonate (0.40 g, 2.85 mmol) and 4-chloro-3-nitrophenacyl bromide (0.35 g, 1.25 mmol) in DMF (5 ml) is stirred at room temperature 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 solid, m.p. 198-200° C. (This compound is also listed as Example 66 in Table 1.)

来源

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