【摘要】 考察了以吡啶-2,6-二甲酸为原料,经酯化、吡啶环自由基亲核取代合成4-羟甲基吡啶-2,6-二甲酸二甲酯的工艺路线,并对吡啶-2,6-二甲酸二甲酯羟甲基化的反应工艺条件进行了优化。结果表明,将9.8 g(44 mmol)吡啶-2,6-二甲酸二甲酯溶于60 mL 30%(V)硫酸和75 mL甲醇混合溶液中,同时等速滴加40.8 mL(400 mmol)30%过氧化氢溶液和含15.2 g(100 mmol)硫酸亚铁的饱和溶液,反应温度控制在30~50℃,目标产物产率可达65.8%,经液相色谱测定产物的纯度大于98%,其结构经由核磁氢谱(1H-NMR),红外分析(IR)和元素分析得以表征。更多还原

【Abstract】 A new procedure for preparing dimethyl 4-(hydroxymethyl)pridine-2,6-dicarboxylate was reported in this paper,in which pyridine-2,6-dicarboxylic acid was used as the starting(material),underwent esterfication and radicals nucleophilic substitution on pyridine ring.The reactive conditions of hydroxymethylation of(dimethyl) pyridine-2,6-dicarboxylate were optimized: in the mixture of (dimethyl) pyridine-2,6-dicarboxylate 9.8 g(44 mmol),60mL solution of 30%(VV) sulphate acid and methanol 75ml,30% hydrogen peroxide 40.8ml(400mmol) and the saturated solution of ferrous sulfate 15.2 g(100 mmol) were added at the same time with the same speed.The reactive(temperature) was kept between 30～50 ℃.The yields of the titled compound can reach 65.8% and(purity) of the product is more than 98% analyzed by HPLC in the above conditions.Un-reacted(starting) material can be used again.The title compound has not been reported in the literatures and its(structure) was characterized by ~1H-NMR,IR,MS and elemental analysis.更多还原