反应 #41261

ord-d13f1c111a6a4d28ac8fdd786615866a

溶剂

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他A small pressure tube equipped with a magnetic stir bar
  2. 2
    其他purging with argon the tube
  3. 3
    其他Crude product was purified by flash chromatography (silica gel, gradient 2 to 10% methanol in dichloromethane), which

实验过程

A small pressure tube equipped with a magnetic stir bar was charged with 100 mg of 2-(4′-bromobiphenyl-4-yl)-4,5-dihydropyridazin-3(2H)-one, 58 mg of (3aR,6aR)-5-methylhexahydropyrrolo[3,4-b]pyrrole dihydrochloride, 350 mg of cesium carbonate, 15 mg of silver triflate, 4.2 mg of tris(dibenzylideneacetone)dipalladium, and 7.2 mg of 2-dicyclohexylphosphino-2′(N,N-dimethylamino)biphenyl and 2 ml of toluene. After sealing and purging with argon the tube was heated at 100° C. for 20 hours. Crude product was purified by flash chromatography (silica gel, gradient 2 to 10% methanol in dichloromethane), which yielded 17 mg of the title compound as a dark yellow oil. Mass spectroscopy gave (M+H)+ m/z 375.2, consistent with assigned structure.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07728031B2uspto-grants-2010_06