摘要
[目的]开发一种绿色合成邻藜芦醛(oV)的工艺。[方法]采用碳酸二甲酯(DMC)作为甲基化试剂,以邻位香兰素为原料,无水碳酸钾为催化剂,合成邻藜芦醛,研究物料配比、反应时间、反应温度和催化剂量对反应的影响。[结果]K2CO3作为催化剂时,oV的选择性和产率最高,分别为78.1%和58.4%。当邻位香兰素和DMC的摩尔比在1.0∶1.3时,邻位香兰素的转化率最大。反应11 h时,oV产率和选择性达到78%和95%。oV的产率和DMC的转化率随温度升高而增加,在150℃时,分别为83%和100%。催化剂最佳用量是K2CO3/邻位香兰素的摩尔比为0.02。[结论]制备oV的最佳工艺条件为:邻位香兰素和DMC的摩尔比为1.0∶1.3,反应时间11 h,反应温度为150℃,K2CO3用量与邻位香兰素摩尔比值为0.02。
[ Objective ] The aim was to develop a kind of process for green synthesis of o-veratraldehyde （oV）. [ Method ] Dimethyl carbonate （DMC） was used as the methylating reagent, o-vanillin as the material and K2CO3 as the catalyzer to synthesize oV. The effect of material ratio, reaction time, reaction temperature and catalyzer dosage on its synthesis reaction was investigated. [Result] When K2CO3 was used as catalyzer, the selectivity and yield rate of oV were the highest, being 78.1% and 58.4% resp. When the molar ratio of o-vanillin to DMC was 1.0：1.3, the translation rate of o-vanillin was the biggest. When the reaction was for 11 h, the yield rote and selectivity of oV reached 78% and 95% resp. The yield rate of oV and the translation rate of DMC were increased with the rise of temperature. At 150 ℃ they were 83% and 100% resp. The optimal amount of was that molar ratio of K2CO3 to o-vanillin was 0.02. [ Conclusion] The optimum process condition to prepare oV was as follows： the molar ratio of o-vanillin to DMC was 1.0：1.3, the reaction time was 11 h, the reaction temperature was 150 ℃ and the molar ratio of K2CO3 amotmt to o-vanillin was 0.02.
出处
《安徽农业科学》
CAS
北大核心
2009年第1期13-15,共3页
Journal of Anhui Agricultural Sciences
基金
江苏省教育厅高校自然科学基金研究项目(06KJB150023)
