摘要
以对氰基苄基氯、邻氨基苯酚和对醛基苯基苯并口恶唑为原料,经加成环化、酯化、缩合三步反应,合成了荧光增白剂双苯并口恶唑二苯乙烯。重点讨论了酯化、缩合两步反应的优化条件,在n(对氯甲基苯基苯并口恶唑)∶n(亚磷酸三乙酯)=1∶4,反应温度165℃,反应时间5h下,酯化收率可达92%;在n(苯并口恶唑基苄基膦酸二乙酯)∶n(对醛基苯基苯并口恶唑)∶n(甲醇钠)=1∶1∶1.6,反应温度20℃,反应时间8h下,缩合收率达到91%以上。双苯并口恶唑二苯乙烯产品纯度大于99%,并用元素分析、红外光谱以及紫外吸收光谱对所得的化合物进行了表征。
4,4′-Bis(2-benzoxazolyl) stilbene,an optical brightener, was synthesized by cyclization, esterification and condensation using 4-cyanobenzyl chloride, o-aminophenol and 4-formylphenylbenzoxazole as raw materials. The optimal conditions of esterification and condensation were discussed. Under the conditions that: n(4-chloromethyl-phenyl-benzoxa-zole)∶n(triethyl phosphite) is 1∶4,reaction temperature is 165℃,and the reaction time is 5 h, the esterification yield is over 92%. Under the conditions that: n(diethyl benzoxazolylbenzyl phosphate)∶n(p-formylphenyl-benzoxazole):n(sodium methylate) is 1∶1∶1.6, reaction temperature is 20℃,and the reaction time is 8 h, the yield of condensation is over 91%. The obtained product was characterized by elementary analysis, IR and UV and its purity is over 99%.
出处
《应用化工》
CAS
CSCD
2005年第5期298-300,共3页
Applied Chemical Industry
