可用于相变材料的顺-4-苯乙烯基吡啶合成研究

Synthesis of Cis-4-styrylpyridine Used for Solid-to-solid Phase Change Material

在乙酸酐存在的条件下,以苯甲醛和4-甲基吡啶进行缩合反应生成了顺-4-苯乙烯基吡啶,探索了反应温度、反应物的物质的量比、反应时间、4-甲基吡啶的加入方式和乙酸酐的用量对产率的影响。确定适宜的反应条件为:30mL乙酸酐,反应温度120～130℃,n(苯甲醛):n(4-甲基吡啶)=1:1.5,4-甲基吡啶以缓慢滴加的方式加入并反应8h,目标化合物的平均收率为40.76%;测得的4-苯乙烯基吡啶的熔点为126.7～127.6℃,差热扫描测得其吸热焓和放热焓分别为52.36J/g和50.43J/g,可通过氢键诱导自组装制备固-固相变储能材料。

Cis-4-styrylpyridine is prepared from benzaldehyde and 4-methylpyridine in the presence of acetic anhydride. Reaction temperature, mole ratio of reactants, reaction time, addition method of 4-methylpyridine and dosage of acetic anhydride on the effect of yield were studied. Optimal reaction conditions are fixed as following: acetic anhydride 30 mL, reaction temperature 120~130 ℃, n(benzaldehyde):n(4-methylpyridine)1:1.5. 4-Methylpyridine is drop added slowly and reacted for 8 hours. The target yield is 40.76%. Melting point of 4 methylpyridine is 126.7~127.6 ℃, exothermic enthalpy and endothermic enthalpy of cis-4-styrylpyridine, which are determined by differential scanning calorimeter, are 52.36 J/g and 50.43 J/g, respectively.