摘要
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。
Investigation has been made on the process for synthesis of salicylaldehyde using phenol,anhydrous magnesium chloride,triethylamine and paraformaldehyde as starting materials.Improvements were made as follows.According to the characteristics of the reaction,the process was divided into two steps.Firstly,magnesium phenoxide was prepared from phenol and magnesium dichloride.Then paraformaldehyde was added.The results showed that the optimal conditions were as follows:The molar ratio of phenol,paraformaldehyde,anhydrous magnesium chloride and triethylamine was 1∶3∶1.5∶1.5;THF was used as the solvent;and a gradual heating process was adopted,with the reaction time proceeded for three hours.The total yield of salicylaldehyde was 73.0% with its purity reaching 99.5% without formation of isomers.
出处
《化学试剂》
CAS
CSCD
北大核心
2011年第2期182-184,共3页
Chemical Reagents
关键词
超声波
苯酚
甲酰化
水杨醛
ultrasonic
phenol
formylation
salicylaldehyde
