摘要
提出了一种合成富马酸二甲酯（ＤＭＦ） 的新方法。以糠醛为原料，先用氯酸钾作氧化剂氧化制得富马酸，再用磷钨酸作催化剂与甲醇进行酯化制得富马酸二甲酯，总产率可达７３％ 。研究了催化剂用量、原料配比、反应温度、反应时间对产率的影响。确定了最佳工艺条件：（１） 糠醛１０ ｍＬ，氯酸钾２５ ｇ，五氧化二钒０－１ ｇ，在１０５ ℃下，搅拌回流反应４ ｈ，富马酸的产率可达８２％ ；（２） 富马酸５ ｇ，甲醇１０ ｍＬ，磷钨酸１－５ ｇ，回流反应４ ｈ，ＤＭＦ的产率可达８９ ％ 。
A new method of synthesis of dimethyl fumarate was given.Furfural was used as the raw material with potassium chlorate as the oxidant to prepare fumaric acid, which was then esterified with methyl alcohol using phosphotungstic acid as the catalyst to produce dimethyl fumarate. The overall yield was up to 73%. The effects of the quantity of the catalyst, ratio of reactants, reaction temperature, and reaction time were studied. The optimum conditions were as follows: (1)a mixture of 10mL furfural,25g potassium chlorate and 0 1g vanadium pentoxide was agitated and refluxed for 4h at 105℃;the yield of fumaric acid was 82%, (2)a mixture of 5g fumaric acid , 10mL methyl alcohol and 1 5g phosphotungstic acid was refluxed for 4h, the yield of DMF was 89%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2000年第1期4-6,共3页
Fine Chemicals
