反应 #640517

ord-c78df7d1d5484863996bbb6f3f6d8280

反应方程式

Nc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Br)cc1
4-[1-(4-bromophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine
O=C([O-])O.[Na+]
sodium bicarbonate
Cl.NO
hydroxylamine hydrochloride
Nc1nonc1-c1nc2ccccc2n1CC(=NO)c1ccc(Br)cc1
title compound
Nc1nonc1-c1nc2ccccc2n1CC(=NO)c1ccc(Br)cc1
4-[1-(4-Bromophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine oxime

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度is refluxed for 20 hours
  2. 2
    其他Partitioning of the reaction mixture between ethyl acetate and water, separation of the organic phase
  3. 3
    其他by drying
  4. 4
    其他evaporation of the solvent
  5. 5
    其他gives the crude product
  6. 6
    其他Purification by chromatography on silicagel

实验过程

A mixture of 4-[1-(4-bromophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine (0.083 g, 0.21 mmol, prepared according to Example 1), sodium bicarbonate (0.021 g, 0.25 mmol) and hydroxylamine hydrochloride (0.014 g, 0.21 mmol) in ethanol (5 ml) is refluxed for 20 hours. Partitioning of the reaction mixture between ethyl acetate and water, separation of the organic phase followed by drying and evaporation of the solvent gives the crude product. Purification by chromatography on silicagel yields the title compound as an E/Z-mixture, m.p. 198-201° C.

来源

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