4-(5-甲酰基-2-甲氧基苯氧基)苯甲酸甲酯化合物的合成  

Synthesis of methyl 4-(5-formyl-2-methoxyphenoxy)benzoate

作　　者：刘德秀[1] 姜娟[2] 娄红祥[2] 

机构地区：[1]苏州卫生职业技术学院,江苏苏州215009 [2]山东大学药学院,山东济南250002

出　　处：《化学试剂》2012年第12期1130-1132,共3页Chemical Reagents

基　　金：国家自然科学基金重点项目(30730109)

摘　　要：4-(5-甲酰基-2-甲氧基苯氧基)苯甲酸甲酯是活性天然产物双联苄全合成的重要中间体,本研究以对溴苯甲酸甲酯和异香兰素为原料,经过缩合反应生成标题化合物,并考查了催化剂、缩合剂、混合缩合剂的比例和反应时间等实验条件对反应产率的影响。结果表明,当催化剂为氧化铜,缩合剂为混合碳酸钙和碳酸钾时,反应产率较理想,其最佳投料比例为n(异香兰素):n(对溴苯甲酸甲酯):n(碳酸钙):n(碳酸钾):n(氧化铜)=1:1.05:0.4:1.6:0.3,反应时间为16 h。Methyl 4-（ 5-formyl-2-methoxyphenoxy ） benzoate was one of the most important intermediate for the total synthesis of bishibenzyls, which is a series of natural products with versatile biological activities. In this work, methyl 4-（ 5- formyl-2-methoxyphenoxy ）benzoate was synthesized from methyl 4-bromobenzoate and iso-vanilline by condensation reaction, and the reaction conditions affecting the yield, such as catalyst,condensing agents, mixed condensing agents and reaction time had been screened. It was found that cupric oxide and the mixture of calcium carbonate with potassium carbonate was the best catalyst and condensing agent, respectively. The best material inputting ratio was proved as follows：n（ isovanilline） ： n （ methyl 4-bromobenzoate ） ： n （ calcium carbonate） ： n （ potassium carbonate ） ： n （ cupric oxide ） = 1 ： 1.05 ： 0. 2： 0. 8： 0. 3 ,The reaction time is about 16 hours.

关 键 词：4-(5-甲酰基-2-甲氧基苯氧基)苯甲酸甲酯 ULLMANN反应 缩合剂 

分 类 号：O625[理学—有机化学]