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探索了在超声波辐射下,以苯酚、多聚甲醛、无水氯化镁和三乙胺为原料合成标题化合物的工艺路线。重点考察了原料配比、温度及加热方式、溶剂种类对反应收率的影响。确定了最佳反应条件为:n(苯酚)∶n(多聚甲醛)∶n(无水氯化镁)∶n(三乙胺)=1∶3∶1.5∶1.5;四氢呋喃为溶剂;采用逐步加热方式;反应时间3 h。在该条件下水杨醛收率可达73.0%,纯度99.5%,无同分异构体产生。
The technological route of synthesizing the title compound with phenol, paraformaldehyde, anhydrous magnesium chloride and triethylamine under ultrasonic irradiation was explored. Focus on the raw material ratio, temperature and heating methods, the impact of solvent types on the reaction rate. The optimal reaction conditions were determined as follows: n (phenol): n (paraformaldehyde): n (anhydrous magnesium chloride): n (triethylamine) = 1: 3: 1.5: 1.5; tetrahydrofuran as solvent; ; Reaction time 3 h. In this condition salicylaldehyde yield up to 73.0%, purity of 99.5%, no isomers.