摘要
以氰乙酸乙酯为起始原料,经氨解反应、加成缩合反应和水解脱羧反应三步合成了β-甲基戊二酸,总收率为77%。对各步反应条件做了优化,开发了一条原料易得、操作简单、收率高、溶剂可循环使用、环境污染小的β-甲基戊二酸合成工艺路线,适于批量生产。采用间接法通过GC-MS分析了水解脱羧反应得到的β-甲基戊二酸和所含杂质,从而探讨了该反应的机理。
β-Methylglutaric acid was synthesized through three steps of ammonolysis,addition-condensation,hydroxylation-decarboxylation by using ethyl cyanoacetate as a raw material,the overall yield was 77%.Conditions of every step was optimized.The process was easy to gain materials,simple operation,high yield,solvent reusing,low environmental pollution and suitable to scale production.The product and by-product of hydroxylation-decarboxylation were analysed using indirect method by GC-MS and the possible mechanism was discussed.
出处
《化学研究与应用》
CAS
CSCD
北大核心
2011年第8期1111-1116,共6页
Chemical Research and Application