반응 #640517

ord-c78df7d1d5484863996bbb6f3f6d8280

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도is refluxed for 20 hours
  2. 2
    기타Partitioning of the reaction mixture between ethyl acetate and water, separation of the organic phase
  3. 3
    기타by drying
  4. 4
    기타evaporation of the solvent
  5. 5
    기타gives the crude product
  6. 6
    기타Purification by chromatography on silicagel

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE042890E1uspto-grants-2011_11