石油化工2013，Vol.42Issue(1)：59-63,5.
3-氰基苯甲酸甲酯的绿色合成
Synthesis of Methyl 3-Cyanobenzoate by a Green Process
摘要
Abstract
Methyl 3-cyanobenzoate was synthesized from methyl 3-formylbenzoat and hydroxylamine hydrochloride by a green method including oximation reaction and dehydration reaction. The effects of sodium hydroxide dosage, solvent ethanol dosage, hydroxylamine hydrochloride dosage, dehydrating agent type and dosage and reaction temperature on the yield of methyl 3-cyanobenzoate were investigated. The end product was identified as methyl 3-cyanobenzoate by means of FTIR and 1 H NMR. The experimental results showed that under the optimum conditions of acetic anhydride as the dehydrating agent, n(methyl 3-formylbenzoate) : n(hydroxylamine hydrochloride) : n(sodium hydroxide) : n(ethanol) : n(acetic anhydride) 1.0 : 1.5 : 1.8 : 6.0 : 1.5 and dehydration temperature 130-140 ℃., the yellow crystal product with the purity higher than 98%(w) could be obtained by succedent washing, filtration and recrystallization with methanol, and the yield of methyl 3-cyanobenzoate could reach 95.1%.关键词
3-醛基苯甲酸甲酯/3-氰基苯甲酸甲酯/肟化反应/脱水反应Key words
methyl 3-formylbenzoate/ methyl 3-cyanobenzoate/ oximation reaction/ dehydration reaction分类
化学化工引用本文复制引用
阮华屹,张旺喜,徐保明,唐强..3-氰基苯甲酸甲酯的绿色合成[J].石油化工,2013,42(1):59-63,5.基金项目
科技部科技人员服务企业项目(2009GJD10016) （2009GJD10016）
湖北省教育厅产学研重大项目(CXY2009A010) （CXY2009A010）
湖北省自然科学基金重点项目(2010CDA020). （2010CDA020）
