新型双(β-二酮)配体的合成研究

Synthesis of Novel Bis-β-diketonate Ligand

以1,6-己二酸为起始物,合成得到噻吩-2,5-二甲酯,经醇化得到噻吩-2,5-二甲酸二甲酯,然后经过Claisen缩合反应得到了新型双(β-二酮)配体。并对它的合成条件分别进行了探索性实验,确定了合成它的各自优化条件。实验结果表明,在以THF为溶剂,噻吩-2,5-二甲酸二甲醇、2-乙酰基噻吩与金属钠的摩尔比为1:4.2:4.2的条件下,把溶解于THF中的2-乙酰基噻吩滴加到噻吩-2,5-二甲酸二甲酯的THF溶液中进行反应,控制反应温度40～45℃,产物双(β-二酮)配体的收率可达65.7%。产品通过元素分析、1HNMR、IR和MS进行组成和结构表征。

The novel bis-β-diketonate ligand was synthesized by esterification and Claisen condensation reaction using thienyl-2,5-dicarboxylic acid as starting material and the Claisen reaction conditions were investigated in detail.The experimental results showed that the product was bis-β-diketonate ligand and its yield was more than 65.7% under the reaction conditions of molar ratio of 2,5-dicarboxythiophene dimethyl ester to 2-acetylthiophene and sodium 1：4.2：4.2,adding 2-acetylthiophene THF solution into 2,5-dicarboxythiophene dimethyl ester THF solution,and reaction temperature of 40～ 45℃.The structures of the compounds were confirmed by IR,1H NMR,MS and elemental analysis.