반응 #219180
ord-fb5162e2dbda41d3b43e92eb53d22fa5
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도is refluxed for 20 hours
- 2기타Partitioning of the reaction mixture between ethyl acetate and water, separation of the organic phase
- 3기타by drying
- 4기타evaporation of the solvent
- 5기타gives the crude product
- 6기타Purification 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.