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α-酮酸酯是重要的有机合成中间体。前文报道了以Grignard试剂与草酸二乙酯反应,合成一系列脂肪族α-酮酸酯的方法。为了进一步了解和掌握这一方法,我们研究了合成4-二甲胺基苯酰甲酸乙酯(1)的反应。1的收率随反应温度、溶剂及原料配比的不同而有显著差别。在本文报道的条件下,收率高达90%。此外,从反应混合物中还分得了2-羟基-2,2-双(对-二甲胺基苯基)乙酸乙酯(2),4,4’-双(二甲胺基)-二苯基乙二酮(3),2-羟基-1,2,2-三(对-二甲胺基苯基)乙酮(4)及4,4’-双(二甲胺基)联苯(5)等副产
Alpha-keto esters are important organic synthesis intermediates. In the previous report, Grignard reagent was reacted with diethyl oxalate to synthesize a series of aliphatic α-keto esters. In order to further understand and master this method, we studied the synthesis of ethyl 4-dimethylaminobenzoate (1) reaction. 1 yield with the reaction temperature, solvent and the ratio of raw materials are significantly different. Under the conditions reported in this paper, the yield is as high as 90%. In addition, 2-hydroxy-2,2-bis (p-dimethylaminophenyl) acetate (2), 4,4’-bis (3), 2-hydroxy-1,2,2-tris (p- dimethylaminophenyl) ethanone (4) and 4,4’-bis (dimethylamino) biphenyl 5) and other by-products