Electric Literature of 2789-89-1,Some common heterocyclic compound, 2789-89-1, name is 1,2-Bis(4-bromophenyl)ethyne, molecular formula is C14H8Br2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
The starting material 2-aminobenzamide (0.3 mmol, 1 equiv),4,4′-dibromodiphenylacetylene (0.9 mmol,3equiv), catalyst palladium trifluoroacetate (Pd(TFA) 2, 0.03 mmol, 10%) and ligand 2,2′-bipyridine (bpy,0.06mmol, 20%) was added to the reaction vessel, and the reaction vessel was continuously subjected to three pumping-oxygenation operations, and then continued.The reaction solvent 1,4-dioxane (1,4-dioxane, 0.4 mL) was added to the reaction vessel, followed by reaction at 100 C in an oil bath.Stir at temperature until the end of the reaction (about 12h), then spin off the reaction solvent and pass column chromatography (filled with 300 mesh in column)400 mesh silica gel, separated by dichloromethane and ethyl acetate in a volume ratio of 10:1 as an eluent), after separation and purification, whiteSolid, yield 79%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,2-Bis(4-bromophenyl)ethyne, its application will become more common.
Reference:
Patent; Wenzhou University; Liu Miaochang; Liu Wei; Bi Kang; Zhu Xiaobin; Gao Wenxia; Huang Xiaobo; Wu Huayue; (11 pag.)CN108129402; (2018); A;,
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