摘要
以2-(2-羟基-5-甲基苯基)苯并三唑、聚缩醛和哌嗪为原料,在乙二醇二甲醚溶剂中,经Mannich反应合成1,4-二[2-(2-羟基-5-甲基苯基)苯并三氮唑]哌嗪,确定了较佳缩合工艺条件。考察了物料配比、反应温度和时间对反应收率的影响,并经过正交实验,确定了反应的最佳工艺条件:在乙二醇二甲醚溶剂中,反应温度95℃,反应时间为24 h,n(2-(2-羟基-5-甲基苯基)苯并三唑)/n(HCHO)/n(哌嗪)=1.0∶1.5∶0.7,产品收率为82%,纯度>98%(HPLC面积归一化法)。产品结构经IR、MS和1H-NMR表征。
In ethylene glycol dimethyl ether solvents, With 2-(2-Hydroxy-5-methylphenyl)benzotriazole, piperazine and paraformaldehyde as raw materials, have a synthesis of 1,4-2[2-(2-hydroxy-5-methyl phenyl) benzene and three azole nitrogen] piperazine by the Mannich reaction, a better condensation process conditions were determined.Inspected the material ratio, reaction temperature and influencing of time on the yield of reaction, the optimum reaction conditions were determined by the orthogonal experiment: In ethylene glycol dimethyl ether solvents, reaction temperature 95 ~C, the reaction time of 24 h, n (uv-P)/n (experiment)/n (piperazine)= 1.0 : 1.5 : 0.7, the product yield was 82%, the purity was 98% (by HPLC area normalization method). Product structure was characterized by IR, MS and ^1H-NMR.
作者
许浩然
王海洋
徐林
陈兴
马赛勇
王守凯
XU Hao-ran WANG Hai-yang XU Lin CHEN Xing MA Sai-yong WANG Shou-kai(Sinosteel Anshan Research Institute of Thermo-energy Co., LTD, Anshan 114001, China)
出处
《广州化学》
CAS
2016年第5期1-6,共6页
Guangzhou Chemistry