3-羟基-2-萘甲酰腙的合成研究

Study on the Synthesis of 3-hydroxy-2-naphthyl Hydrazone

以3-羟基-2-萘甲酸、水合肼、甲醇、甲基异丁基酮为原料,经三步法(酯化反应、酰肼化反应、酰腙化反应)合成高纯度的目标产物3-羟基-2萘甲酰腙。考察了原料配比、催化剂种类、酯化反应时间、温度等对各反应速率的影响。结果表明,醇酸比为4,催化剂为浓硫酸时,酯化反应更加充分;肼酯比为4时,更有利于酰肼化反应进行;温度为85℃酰腙化反应更加完全。该方法反应条件温和、操作步骤简单,所得产品收率高。

Using 3-hydroxy-2-naphthalic acid,hydrazine hydrate,methanol and methyl isobutyl ketone as raw materials,high-purity target product 3-hydroxy-2 naphthaloyl hydrazone is synthesized by three-step method cesterification,hydrazidation,hydrazone.The effects of raw material ratio,catalyst type,esterification time and temperature on the reaction rate are investigated.The results show that when the ratio of alcohol to acid is 4 and the catalyst is concentrated sulfuric acid,the esterification reaction is more sufficient.When the hydrazine ester ratio is 4,the hydrazidation reaction is more favorable.Acylhydrazone reaction is more complete at 85℃.The method has mild reaction conditions,simple operation steps and high yield.