3-(2,4-二甲基-3-戊氧基)邻苯二腈的合成

Synthesis of 3-(2,4-dimethyl-1-pentenyl-3-oxy)-phthalonitrile

以3-硝基邻苯二腈、2,4-二甲基-3-戊醇、氢化钠为原料,进行赖因德斯—林格反应缩合,合成目标化合物——3-(2,4-二甲基-3-戊氧基)邻苯二腈,主要探讨了原料摩尔比、反应温度、滴加时间对产品质量和收率的影响。确定了较优反应条件;3-硝基邻苯二腈与2,4-二甲基-3-戊醇钠的摩尔比为1∶1.25,反应温度为0℃,滴加时间为3 h,反应时间2 h,反应收率为87%。通过熔点,HNMR确证目标产物的化学结构。

3 - （2,4 - dimethyl - 1 - pentenyl - 3 - oxy） - phthalonitrile was synthesized by Reinders - Ringer reaction of 3 - Nitrophthalonitrile, 2,4 - dimethyl - 3 - pentanol, Sodium hydride. The mole ratio of raw material, reaction tempera- ture, adding time to product quality and yield of influence were mainly discussed. The optimum conditions were as follows ： 3 - nitrophthalonitrile and B mole ratio of 1 ： 1.25, and the reaction temperature was 0℃, the adding time was 3 h, the reaction time was 2 h, the reaction yield was 87%. The target product was characterized by the melting point and HNMR.