α-联苯双酯的合成工艺优化

Optimization of Synthesis Technology of α-Dimenthoxy Dicarboxylate Biphenyl

以3,4-二羟基-5-甲氧基苯甲酸甲酯为原料,经溴化、环合、乌尔曼反应合成了α-联苯双酯(-αDDB)。该反应过程经改进后,符合准一步反应原则和不提纯原则。经正交试验得到的最佳实验条件:溴素用量6.8 mL,二氯甲烷175 mL,碳酸钾6 g,环合反应温度90℃,铜粉用量15 g,乌尔曼反应温度145℃。在此条件下,三步反应总收率达到66.1%,比目前工艺提高了8.7%,产品纯度达99%以上。

α-Dimenthoxy dicarboxylate biphenyl（α-DDB） was synthsized from 3, 4-di- hydroxy-5-methoxy methyl benzoate through bromination reaction, cyclization reaction and ullmann reaction. The improved technology accorded with similar one step reaction and non-purification principles. The optimum technology conditions were determined by orthogonal tests,as follows： the dosages of bromine 6.8 mL, dichloromethane 75 mL, potassium carbonate 6 g,cuprum were 15 g,the temperature of cyclization reaction 90℃ and ullmann reaction 145℃. Under these conditions, the total yield reached 66. 1%, increasing about 8.7 % comparing with the current technology. Furthermore the purity of the product was over 99%.