石油化工2012，Vol.41Issue(11)：1293-1297,5.
分步法合成藜芦醚工艺的研究
A Two-Step Synthesis Method for o-Dimethoxy Benzene
摘要
Abstract
The synthesis of o-dimethoxy benzene from catechol(CA) and dimethyl sulfate(DMS) by a two-step methylation process with NaOH aqueous solution as the condensation agent under nitrogen protection which prevented catechol from being oxidated in air was investigated. The effects of water and methanol as the solvents of NaOH on the synthesis were observed, and the results revealed that the product with higher yield and purity were achieved in the NaOH aqueous solution. The influences of the mole ratio of DMS to CA, mass fraction of NaOH solution, reaction time and temperature of the second step reaction on the yield of o-dimethoxy benzene were investigated by orthogonal design. Under the optimal reaction conditions: n(CA) : n(DMS) : n(NaOH) 1.00 : 2.45 : 2.57, the mass fraction of NaOH 16.67%, temperature 80 ℃ and reaction time 3 h in the second step, the total yield of the product o-dimethoxy benzene could reach 95%. The product was characterized by means of 1H NMR.关键词
藜芦醚/邻苯二酚/硫酸二甲酯/甲基化反应Key words
o-dimethoxy benzene/ catechol/ dimethyl sulfate/ methylation分类
化学化工引用本文复制引用
李博,高兴娜,郭翔海,白鹏..分步法合成藜芦醚工艺的研究[J].石油化工,2012,41(11):1293-1297,5.
