摘要
以二苯氨基脲为催化剂,3,4,5-三羟基苯甲酰肼(2)和对羟基苯甲醛(3)通过缩合反应合成了一个新型的酰腙化合物——对羟基苯甲醛-3,4,5-三羟基苯甲酰腙(H2L),其结构和性能经1H NMR,IR,元素分析和TGDTG表征。在最佳反应条件[二苯氨基脲0.12 g(1.58%),2 25 mmol,n(2)∶n(3)=1.0∶1.0,回流反应7 h]下制备的H2L,收率66.85%,初始分解温度为170.06℃,导电率为9.9μs·cm-1。H2L与硝酸锰和吡啶形成的配合物[Mn(LPy)2]溶液的电导率为4.1×102μs·cm-1。
A novel acylhydrazone compound,4-hydroxybenzaldehyde-3,4,5-trihydroxybenzoyl hydrazone(H2L),was synthesized by condensation of 3,4,5-trihydroxybenzoylhydrazine (2) with 4-hydroxybenzaldehyde(3) using 1,5-diphenylcarbazide as the catalyst.The structure and properties were characterized by 1H NMR,IR,elemental analysis and TG-DTG.The optimum reaction conditions refluxed for 7 h were as follows:1,5-diphenylcarbazide was 0.12 g(1.58%),2 was 25 mmol,n(2) ∶ n(3) was 1.0 ∶ 1.0.The yield of H2L was 66.85% under the optimum reaction conditions.The initial decomposition temperature of H2L was 170.06 ℃ and conductivity was 9.9 μs · cm-1.Conductivity of the complex [Mn (LPy) 2],which was obtained by coordination of H2L with Mn (NO3) and pyridine,was 4.1 ×102 μs · cm-1.
出处
《合成化学》
CAS
CSCD
北大核心
2014年第4期489-491,495,共4页
Chinese Journal of Synthetic Chemistry
基金
陕西省自然科学基础研究计划项目(2013JQ6010)
陕西省大学生创新创业项目(201204056)