3,5-二叔丁基-4-羟基苯基丙酸-1-膦-2,6,7-三氧双环-[2,2,2]辛基-4-甲酯的合成新工艺

以 3 - (3 ,5 -二叔丁基 - 4-羟基苯基 )丙酸甲酯 (简称 3 ,5 -甲酯 )、亚磷酸三乙酯、季戊四醇为原料 ,二丁基氧化锡为催化剂合成了标题化合物。考查了催化剂、反应温度、反应时间及物料配比等因素的影响 ,实验结果表明 :以 0 .1 mol季戊四醇为准 ,第一步和第二步反应温度分别为 1 1 0～ 1 2 0°C和 1 40°C,催化剂用量为 0 .6 g,反应时间为 5 h,n(季戊四醇 )∶n(亚磷酸三乙酯 )∶n(3 ,5 -甲酯 ) =1∶ 1∶ 1 .1 0 ,在此条件下 ,收率在 95 %以上。通过元素分析、红外光谱分析、核磁氢谱对产品进行组成结构表征

New Synthesis Method of 3,5-Ditertbutyl-4-hydroxyphenyl- propionic acid-1-phospho-2,6,7-trioxabicyclo- [2,2,2]octyl-4-methylester

diterbutyl 4 hydroxyphenyl propionic acid 1 phospho 2,6,7 trioxabicyclo [2,2,2]octyl 4 methylester was prepared by the transesterification reaction of tetramethylol methane, triethyl phosphite and methyl 3 (3,5 ditertbutyl 4 hydroxyphenyl) propionate (abbreviated to 3,5 methylester) using an organic tin compound as the catalyst. The affects of catalyst, temperature, reaction time and molar ratio of the raw materials on the reaction were studied. The experimental results showsed that the optimum conditions were as follows: reaction temperature of the first step and the second step separately were 110～120 °C and 140 °C , respectively, the catalyst load was 0.6 g, the reaction time was 5 h, and the molar ratio of the above listed substantces was 1∶1∶1.10 (based on 0.1 mol tetramethylol methane). Under these conditions, the yield of the product can be above 95%. The composition and structure of the product were characterized by elemental analysis, IR, and 1H NMR.