摘要
以磷钨酸为催化剂,通过香兰素与1,2-丙二醇反应合成了标题化合物。研究了原料配比、反应时间、催化剂的种类和用量、带水剂的种类以及催化剂重复使用后对收率的影响。并研究了磷钨酸催化其他的醛酮与醇的缩合,实验表明,磷钨酸是催化合成缩醛(酮)的理想催化剂,其较优反应条件为:n(香兰素)∶n(1,2-丙二醇)=1∶1.3,催化剂用量为反应物总质量的0.3%,带水剂为15 mL苯,回流反应2 h,活性98%以上,收率达94.58%以上。通过GC1、HNMRI、R等数据对所合成的目标产物进行了表征。
Vanillin 1,2-propylene glycol acetal was synthesized from vanillin and 1,2-propylene glycol using H3PMo12O40 as the catalyst. Factors influencing the yield, such as the molar ratio of starting materials, time, catalyst species and amount, and different water entraining agents, were studied and the better reaction conditions were determined. The factors influencing the synthesis were studied and the optimal reaction conditions were found as follows：a molar ratio of cinamaldehyde /ethylene glycol = 1.0/ 1.3, a catalyst dosage of 0.3 %, a cyclohexane amount of 15 mL, and a reaction time of 4.5 h. The selectivity was above 98 % and the product yield was 94.58%. The structure of vanillin 1,2- propylene glycol acetal was identified by means of IR, GC and ^1HNMR.
出处
《化学试剂》
CAS
CSCD
北大核心
2009年第6期457-460,共4页
Chemical Reagents
关键词
香兰素缩1
2-丙二醇
香兰素
1
2-丙二醇
磷钨酸
绿色催化
合成
vanillin 1,2-propylene glycol acetal
vanillin
1,2- propylene glycol
H3PMo12O40
green catalyze
synthesis
