摘要
以邻氨基苯甲醚为原料,经重氮化、水解、甲基化的方法合成邻苯二甲醚,最佳反应条件为:n(邻氨基苯甲醚)∶n(硫酸)∶n(亚硝酸钠)=1.0∶3.0∶1.01,n(邻羟基苯甲醚)∶n(硫酸二甲酯)=1∶1.4,重氮化温度为10～15℃,水解时酸的浓度为40%,水解温度为110℃;甲基化温度为80℃,反应时间3h,总收率为84.8%。产物用红外光谱、核磁共振等进行了表征。
o-Dimethoxy benzene was prepared from oanisidine by diazotization,hydrolysis and methylation.The optimal reaction conditions were as follows：n（o-anisidine）∶n（sulfuric acid）∶n（sodium nitrite）=1.0∶3.0∶1.01,n（ohydroxy methylphenate）∶n（dimethyl sulfate）=1∶1.4,the diazotization temperature was 10～15℃,the acid concentration and temperature in process of hydrolysis were 40% and 110℃ respectively;the methylation temperature was 80℃,the reaction lasted 3h and the total yield was 84.8%.The product was confirmed by IR and 1HNMR.
出处
《精细与专用化学品》
CAS
2007年第24期16-18,共3页
Fine and Specialty Chemicals
