【摘要】 以四氯化碳和乙烯基乙醚为原料,在引发剂作用下发生自由基加成反应制备1,1,1,3-四氯-3-乙氧基丙烷(以下简称丙烷化合物),丙烷化合物与甲醇回流得到3,3-二甲氧基丙酸甲酯,然后在裂解催化剂的作用下裂解为3-甲氧基丙烯酸甲酯。优化工艺条件为:催化剂为偶氮二异丁腈/间氯过氧苯甲酸,n(乙烯基乙醚)∶n(四氯化碳)∶n(偶氮二异丁腈)∶n(间氯过氧苯甲酸)=1∶1.6∶0.001 6∶0.001 6,反应温度为68℃,反应时间为6 h;裂解反应所用催化剂为对甲苯磺酸。3步反应总收率为67.7%(以乙烯基乙醚计),含量为98.5%。更多还原

【Abstract】 Methyl 3-methoxyacrylate was pyrolyzed by methyl 3,3-dimethoxy-propionate, which was successfully synthesized from the reflux of 1,1,1,3-tetrachloro-3-ethoxy-propane in methanol. 1,1,1,3-tetrachloro-3-ethoxypropane was prepared using vinyl ether and carbon tetrachloride as the raw materials, AIBN and 3-chloroperbenzoic acid as catalysts. The optimum conditions for synthesis of 1,1,1,3-tetrachloro-3-ethoxypropane were as followings: n(vinyl ether):n(carbon tetrachloride):n(AIBN):n(3-chloroperbenzoic acid) was of 1:1.6:0.0016:0.0016; reaction temperature was of 68℃; reaction time was of 6 h; the cracking catalyst was p-toluenesulfonic acid. The overall yield of the target compound reached 67.7% with a purity of 98.5%.更多还原