反応 #219180

ord-fb5162e2dbda41d3b43e92eb53d22fa5

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07385061B2uspto-grants-2008_06