酸酐法合成乙酸酯类物质的一种新型催化体系的研究

Study on A New Catalytic System for Synthesis of Acetate by Anhydride Method

以DMAP+I2作为催化体系,考察了其在叔丁醇与乙酸酐的酰化反应中的催化性能,实验结果表明,该催化剂可使乙酸酐与高位阻的叔丁醇顺利进行酯化反应,乙酸叔丁酯收率可高达70%以上,并且反应条件温和、催化体系易被回收和重复使用。同样通过实验验证该催化体系也可高效作用于正丁醇、仲丁醇与乙酸酐的反应。DMAP+I2催化体系经核磁共振、质谱仪进行表征分析,发现DMAP和碘单质之间发生了配位或者酸碱反应,重复反应多次,催化剂组分没有发成改变。

The acylation of tert-butanol with acetic anhydride was studied by using DMAP doped with iodine as catalysts.The experiment results showed that DMAP doped with iodine had a good catalytic activity for the acylation of tert-butanol with acetic anhydride.The yield of tert-butyl acetate was up to more than 70%.The reaction conditions were mild and the catalytic system was easy to be recycled and reused.Similarly,the catalytic systems can also effectively catalyze the acylation of n-butanol and sec-butanol with acetic anhydride.The catalytic system of DMAP+I 2 was characterized by NMR and mass spectrometry.It was found that coordination or acid-base reaction took place between DMAP and iodine.The catalyst composition remained unchanged after repeated reactions.