摘要:
The key intermediate of Angustifolin D, 6,6′-bis[(Z)-2-iodoprop-1-en-1-yl]-2,2′,3,3′, 4 ,4′-hexamethoxy-1 ,1′-biphenyl ( 7 ) , was synthesied by six steps reaction with an overall yield of 23% from 3,4,5-trimethoxybenzoic acid. The structure was confirmed by 1 H NMR, 13 C NMR, IR and MS. The biaryl coupling reation as the key step was achieved using an atropdiastereoselective oxidative ( CuBr·SMe2 ) as the catalyst.%以3,4,5-三甲氧基苯甲酸为原料,经6步反应以23%总收率完成了Angustifolin D关键中间体———6,6′-2[(Z)-2-碘代-1-丙烯基]-2,2′,3,3′,4,4′-六甲氧基-1,1′-联苯(7)的合成,其结构经1H NMR,13C NMR, IR和MS确证。其中关键步骤联苯偶连反应采用了廉价易得的铜试剂( CuBr·SMe2)作为催化剂。