摘要
以晶体乙醛酸和尿素为原料经环化缩合合成了尿囊素。考察了溶剂种类、混合溶剂摩尔比、催化剂种类、原料摩尔比、反应时间对产品收率的影响。结果表明:溶剂的极性太强或太弱对反应都不利,选择四氢呋喃和乙醇的混合溶液为反应溶剂;n(四氢呋喃)∶n(乙醇)=1∶1.5,4.4 g的H2SO4和H3PO4作催化剂(摩尔比1∶1),n(乙醛酸)∶n(尿素)=1∶4,反应温度75℃、时间4 h时,尿囊素产率85.4%,产品纯度98.9%。尿囊素的结构用FT-IR1、H NMR和13C NMR进行了表征。
Allantoin was synthesized als by cyclization and condensation solvent, catalyst kind, molar ratio using crystal glyoxylic acid reactions. The effects of sol and urea as raw vent of reactant and reaction time on kind, reactio molar materlratio of n results were examined. The results showed that the mixture of tetrahydrofuran and ethanol was a suitable solvent for the reaction and the yield of product was 85.4% with the purity of more than 98.9 G under the following conditions:n(tetrahydrofuran) : n(ethanol) = 1: 1.5, n(glyoxylic acid) : n(urea)= 1 : 4, reaction time 4 h in the presence of mixture of sulfuric acid and phosphoric acid as catalyst. The structure of obtained product was characterized by FT-IR,^1H NMR and ^13C NMR.
出处
《青岛科技大学学报(自然科学版)》
CAS
2008年第2期106-109,共4页
Journal of Qingdao University of Science and Technology:Natural Science Edition
关键词
乙醛酸
尿囊素
溶剂
合成
glyoxylic acid: allantoin
solvent
synthesis