【摘要】 以异香兰素为原料,经O-烷基化反应和氰基化反应制备医药中间体3-乙氧基-4-甲氧基苯腈,考察了O-烷基化反应和氰化反应的影响因素。实验表明:制备3-乙氧基-4-甲氧基苯甲醛的最佳合成工艺条件为:异香兰素45.6g(0.30mol),n(异香兰素)∶n(溴乙烷)=1∶1.15,0.5 MPa于85℃反应5h,3-乙氧基-4-甲氧基苯甲醛的收率达到97%以上;以3-乙氧基-4-甲氧基苯甲醛为原料,经氰化反应制备3-乙氧基-4-甲氧基苯腈的最佳工艺条件为:在乙酸介质中,3-乙氧基-4-甲氧基苯甲醛与盐酸羟胺的摩尔比为1.0∶1.5,于70~80℃下反应4h,3-乙氧基-4-甲氧基苯腈的收率超过91%,纯度99.4%。更多还原

【Abstract】 The methods for preparing 3-ethoxyl-4-methoxybenzene nitrile have been studied by o-alkylation reaction and cyanidation of isovanillin.The effects on O-alkylation reaction and cyanidation reaction were investigated.Experiments show that the optimum synthetic process conditions for preparation of 3-ethoxy-4-methoxy benzaldehyde:isovanillin 45.6 g(0.30 mol),isovanillin and bromine ethane mole ratio was 1∶1.15,after 5 h,the yield of 3-ethoxy-4-methoxy benzaldehyde reached above 97%at 0.5 MPa and 85℃;3-ethoxy-4-methoxy benzaldehyde as raw material,optimum technological conditions for preparation of 3-ethoxyl-4-methoxybenzene nitrile by cyanide reaction were:in acetic acid medium,3-ethoxy-4-methoxy benzene,formaldehyde and hydroxylamine hydrochloride mole ratio 1.0∶1.5,after 4 h,3-ethoxyl-4-methoxybenzene nitrile yield more than 91%,the purity of 99.4% at 70-80 ℃.This method has following advantages:mild reaction conditions,cheap raw materials,high yield,good purity and suitable for industrial production.更多还原