顺式-2-甲氧亚胺基-2-呋喃乙酸合成工艺研究

The Technologic Research for the Synthesis of Syn-2-(2-furyl)-2-(methoxyimino)acetic Acid

以2 呋喃甲酸为起始原料,经氯代、氰代、水解、肟化合成了顺式 2 甲氧亚胺基 2 呋喃乙酸。改进了氰代反应方法,其主要反应条件为n(2 呋喃甲酸)∶n(氯化亚砜)=1∶2 5,n(2 呋喃甲酰氯)∶n(氰化亚酮)=1∶2,n(2 氧代 2 呋喃乙酸)∶n(甲氧基胺盐酸盐)1∶1 2,水解温度为0℃,肟化介质pH值为5～6。顺式 2 甲氧亚胺基 2 呋喃乙酸的总收率达45 9%。用元素分析、1H NMR证明了目标化合物结构正确。

Syn-2-(2-furyl)-2-(methoxyimino)acetic acid is prepared by chlorination,cyanation,hydrolysis and oximation from 2-furancarboxylic acid.The method of cyanation is improved.The major reaction conditions are as follows:mole ratio of n(2-furancarboxylic acid)∶n(SOCl_2)=1∶2.5,n(2-furoy1 chloride)∶n(CuCN)=1∶2,n(2-oxo-2-fury1 acetic acid)∶n(methoxylamine hydrochloride)=1∶1.2,hydrolysis temperature 0℃,pH of oximation 5~6.The overall yield of target compound can reach 45.9%.The structure of the product is identified with element analysis and ~1H-NMR.