• 专利标题:   Graphene-supported nano-palladium-catalyzed carbonyl amination of halogenated aromatic hydrocarbon e.g. iodobenzene, involves extracting graphene-supported nano-palladium catalyst and halogenated aromatic hydrocarbon and amidating.
  • 专利号:   CN104045579-A, CN104045579-B
  • 发明人:   CHEN C, GAO P, GAO Z, SUN H, ZHANG W, ZHANG Y
  • 专利权人:   UNIV SHAANXI NORMAL
  • 国际专利分类:   B01J023/44, C07C231/00, C07C233/65, C07C235/46
  • 专利详细信息:   CN104045579-A 17 Sep 2014 C07C-233/65 201482 Pages: 5 Chinese
  • 申请详细信息:   CN104045579-A CN10260531 12 Jun 2014
  • 优先权号:   CN10260531

▎ 摘  要

NOVELTY - Graphene-supported nano-palladium-catalyzed carbonyl amination of halogenated aromatic hydrocarbon involves ultrasonically-dispersing graphene-supported nano-palladium catalyst in N,N-dimethylformamide, adding halogenated aromatic hydrocarbon, stirring, cooling to room temperature, filtering, pouring filtrate into saturated sodium bicarbonate aqueous solution, extracting with ethyl acetate, drying organic phase using anhydrous magnesium sulfate, concentrating under reduced pressure, purifying, aminating, washing the product using N,N-dimethylformamide and distilled water, and drying. USE - Graphene-supported nano-palladium-catalyzed carbonyl amination of halogenated aromatic hydrocarbon e.g. iodobenzene, p-methoxy-iodobenzene, p-iodobenzene, 1-iodo-naphthalene and bromobenzene (all claimed). ADVANTAGE - The method is environmentally-friendly and enables efficient graphene-supported nano-palladium-catalyzed carbonyl amination of halogenated aromatic hydrocarbon, by simple method. DETAILED DESCRIPTION - Graphene-supported nano-palladium-catalyzed carbonyl amination of halogenated aromatic hydrocarbon involves ultrasonically-dispersing graphene-supported nano-palladium catalyst in N,N-dimethylformamide, adding halogenated aromatic hydrocarbon, stirring in Teflon (RTM: polytetrafluoroethylene)-lined stainless steel autoclave at 160-200 degrees C for 12-48 hours, cooling to room temperature, filtering, pouring the filtrate into saturated sodium bicarbonate aqueous solution, extracting with ethyl acetate, drying organic phase using anhydrous magnesium sulfate, concentrating under reduced pressure, purifying using silica gel column chromatography, aminating, washing the product using N,N-dimethylformamide and distilled water, and drying under vacuum. The content of graphene-supported nano-palladium catalyst is 0.001-1 mol%.