石油化工2025，Vol.54Issue(2)：173-178,6.DOI:10.3969/j.issn.1000-8144.2025.02.004
5-氨基-2,4-二羟基苯甲酸的合成工艺优化
Optimization of synthesis process of 5-amino-2,4-dihydroxybenzoic acid
摘要
Abstract
The AB-type monomer 5-amino-2,4-dihydroxybenzoic acid(ADHBA)was successfully synthesized via Kolbe-Schmitt,nitrification,and reduction reactions by using resorcinol as material.The structures of products were characterized by FTIR,1H NMR,and EI-MS,and the synthetic conditions were optimized.The experimental results show that when n(resorcinol)∶n(sodium bicarbonate)is 1∶3,water serves as a solvent,the reaction temperature is 100℃,and the reaction time is 4 h,the purity and yield of 2,4-dihydroxybenzoic acid determined by HPLC are 99.8%and 68.4%,respectively.When n(2,4-dihydroxybenzoic acid)∶n(nitric acid)is 1∶2,acetonitrile serves as a solvent,the reaction temperature is 45℃,and the reaction time is 3.5 h,the purity and yield of 5-nitro-2,4-dihydroxybenzoic acid(DHNBA)determined by HPLC are 99.7%and 60.2%,respectively.When Pd/C and water serve as catalyst and solvent,m(Pd/C)∶m(DHNBA)∶m(water)is 1∶20∶1 000,the pressure of H2 is 0.4 MPa,the reaction temperature is 50℃,and the reaction time is 6 h,the purity and yield of ADHBA determined by HPLC are 98.6%and 73.2%,respectively.关键词
间苯二酚/5-氨基-2,4-二羟基苯甲酸/Kolbe-Schmitt反应/硝化反应/还原反应Key words
resorcinol/5-amino-2,4-dihydroxybenzoic acid/Kolbe-Schmitt reaction/nitrification reaction/reduction reaction分类
化学化工引用本文复制引用
吴弼辰,吴纯鑫,赵德明..5-氨基-2,4-二羟基苯甲酸的合成工艺优化[J].石油化工,2025,54(2):173-178,6.基金项目
江苏省重大科技计划支撑项目(BE2011129) （BE2011129）
浙江省教育厅项目(Y201121211). （Y201121211）
