3,4,5-三甲氧基氯苄的正交优化合成

Synthesis of 3,4,5-trimethoxylbenzyl chloride by orthogonal design

目的:优化合成3,4,5-三甲氧基氯苄的方法。方法:以四氢呋喃为溶剂,3,4,5-三甲氧基苯甲酸在ZnCl2/NaBH4还原体系中制备3,4,5-三甲氧基苄醇,并经正交设计优化合成工艺研究,醇经氯化反应得到3,4,5-三甲氧基氯苄。结果:经过IR、1H-NMR分析,证明产物是3,4,5-三甲氧基氯苄。结论:该工艺可以较高产率地合成3,4,5-三甲氧基氯苄,并且条件温和。

Objective： To study a good method of synthesize 3,4,5-trimethoxylbenzyl chloride.Methods： Used THF as solvent and 3,4,5-trimethoxylbenzene carbonic acid as the raw material,the 3,4,5-trimethoxylbenzyl chloride was prepared by an reduction action in ZnCl2/NaBH4 system,the acid translated into 3,4,5-trimethoxylbenzalcohol,and then by chlorination,the alcohol changed into 3,4,5-trimethoxylbenzyl chloride.Results： The target production was determined by IR and 1H-NMR spectrum.Conclusion： The 3,4,5-trimethoxylbenzyl chloride can be get by this process with high yield in mild condition.