반응 #219180

ord-fb5162e2dbda41d3b43e92eb53d22fa5

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: US07385061B2uspto-grants-2008_06