Reaktion #640517

Reaktionsgleichung

4-[1-(4-bromophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine

sodium bicarbonate

hydroxylamine hydrochloride

→

title compound

4-[1-(4-Bromophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine oxime

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis refluxed for 20 hours
2. 2
   SonstigePartitioning of the reaction mixture between ethyl acetate and water, separation of the organic phase
3. 3
   Sonstigeby drying
4. 4
   Sonstigeevaporation of the solvent
5. 5
   Sonstigegives the crude product
6. 6
   SonstigePurification by chromatography on silicagel

Vorschrift

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.

Quelle