摘要
以—水乙醛酸和尿素为原料,对甲基苯磺酸—磷酸构成的复合酸作为催化剂,利用微波辅助加热技术,经环化缩合反应制备了医药和有机合成中间体及日化助剂尿囊素。研究表明,微波辅助加热可以有效地提高反应效率,反应中的微波辐射功率以500~700W为宜;在微波辐射功率为650W时,微波加热反应15min后尿囊素收率可达60%左右,结果相当于普通加热方式加热反应6h的效果。产品经元素分析、熔点测定、红外光谱表征并用滴定法测定其纯度,尿囊素含量在98%以上。
Allantoin, as the intermediate of organic synthesis and the agent of medical and cosmetics, was prepared from glyoxalic-monohydrate and urea by cyclization and contractile reaction under the present of p-toluenesulfonic acid and phosphosic acid as catalyst and the use of microwave technology. The result indicated that reaction efficient could be improved with the use of microwave in the heating process. The optimum microwave power was 500-700 W. When the microwave power was 650W and the reaction was heated by microwave over 15 min, the yield of allantoin may be up to 60% This result was equaled to that of the reaction was heated by common heating method over 6 h. The product was determined by elementary analysis, IR and melt-point analysis .The purity of product determined by drop scale method was above 98%.
出处
《化工科技市场》
CAS
2005年第11期24-27,共4页
Chemical Technology Market
关键词
尿囊素
微波辅助
催化合成
allantoin
microwave assistance
synthesis by catalysis