2,6-二氟-4-羟基苯甲腈的合成

实验以3,5-二氟苯胺为原料,经溴化、重氮化水解和氰化合成2,6-二氟-4-羟基苯甲腈。重氮化水解步骤的最佳反应条件为:n(4-溴-3,5-二氟苯胺):n(水)=1:30,n(4-溴-3,5-二氟苯胺):n(磷酸)=1:6,n(4-溴-3,5-二氟苯胺):n(五水硫酸铜)=1:1.0。该法生产成本低廉,反应条件温和,适合于工业化生产。产物含量为99%,摩尔产率为21.7%,其结构通过MS和~1H MR进行论文验证。

SYNTHESIS OF 2,6-DIFLUORO-4-HYDROXYBENZONITRILE

It is proposed a synthesized method of 2,6-difluoro-4-hydroxycyanobenzene,which takes 3, 5-difluoroaniline as raw material,followed by bromination,diazotization hydrolysis and cyanidation. The optimal reaction condition of diazotization hydrolysis are:n(4-bromo-3,5-difluoroaniline):n (H_2O) = 1:30,n(4-bromo-3,5-difluoroaniline):n(phosphoric acid) = 1:6 and n(4-bromo-3,5-difluoroaniline) :n(copper sulfate pentahydrate) = 1:1.0.This method has low cost,mild reaction condition,and is suitable for production in industrial scale.Product content is 99%,molar yield is 21.7%,and the structure of product is confirmed by MS and ~1H NMR.