己二醇双[3-(3,5-二叔丁基-4-羟基苯基)]丙酸酯的合成

Synthesis of hexamethylene glycol bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)] propionate

以 3 -(3 ,5 -二叔丁基 -4-羟基苯基 )丙酸甲酯 (简称 3 ,5 -甲酯 )与 1 ,6-己二醇为原料 ,有机锡为催化剂 ,在无溶剂的条件下合成了己二醇双 [3 -(3 ,5 -二叔丁基 -4-羟基苯基 ) ]丙酸酯。通过实验考察了反应温度、催化剂用量、反应时间及物料配比等因素的影响。结果表明 ,最佳的反应条件是反应温度 1 2 0～ 1 40℃ ,催化剂用量为反应物总质量的 1 .2 %左右 ,反应时间 4h,3 ,5 -甲酯与 1 ,6-己二醇摩尔比为 2 .0 5∶ 1。在此条件下 ,收率在 95 %以上 ,并通过元素分析、红外光谱分析。

Hexamethylene glycol bis[3 (3,5 di tert butyl 4 hydroxyphenyl)] propionate was synthesized without solvent with methyl 3 (3,5 di tert butyl 4 hydroxyphenyl) propionate and hexamethylene glycol as raw materials and organic tin as catalyst.The influence of temperature,reaction times,catalyst and the molar ratio of raw materials on the yield of the product were studied.The experimental result shows that the optimum conditions were as follows:reaction temperature is ranged from 120~140℃;the catalyst is 0.4 g,reaction time is 4 h and the molar ratio of methyl 3 (3,5 di tert butyl 4 hydroxyphenyl) propionate and hexamethylene glycol is 2.05∶1.The yield of the product was up to 95% under the optimum conditions.The structure of the product was characterized by elementary analysis,IR,and 1HNMR.