4,4′-二氨基二苯甲烷与碳酸二甲酯甲氧基羰基化制备4,4′-二苯甲烷二氨基甲酸甲酯

Preparation of methyl 4,4′-diphenylmethane dicarbamate by methoxycarbonylation of 4,4′-diaminodiphenylmethane with dimethyl carbonate

研究了4,4′-二氨基二苯甲烷(MDA)与碳酸二甲酯(DMC)甲氧基羰基化合成4,4′-二苯甲烷二氨基甲酸甲酯(MDC)的反应,研究了反应的影响因素,并采用FTIR、1 H NMR等测试方法对合成产物的结构进行了表征。结果表明,合成MDC的最佳反应工艺为反应温度160℃,用醋酸铅催化,且m(醋酸铅)∶m(MDA)=6%,反应物配比n(DMC)∶n(MDA)=20∶1,反应时间3h。在上述反应条件下,MDA的转化率达到100%,MDC的收率达到96.6%。

The reaction of4,4′-diaminodiphenylmethane(MDA)and dimethyl carbonate(DMC)methoxycarbonylation to4,4′-diphenylmethanedicarbamate(MDC)was studied.The influencing factors of the reaction were characterized by FTIR,1H-NMR and other methods.The results show that the optimal reaction process for synthesizing MDC is:reaction temperature is160℃,and m(lead acetate)∶m(MDA)is6%,and the ratio of reactants is n(DMC)∶n(MDA)=20∶1.The reaction time is3h.Under the above reaction conditions,the conversion of MDA reached100%,and the yield of MDC reached96.6%.