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以吡咯和对苯二甲醛为原料,采用无溶剂Michael加成反应一步合成1,4-二(2,2’-二吡咯甲基)苯(BDMP)。考察了投料比、温度、催化剂等因素对反应的影响。得出合成的最佳工艺条件为:n(吡咯)∶n(对苯二甲醛)∶n(丙酸)=4∶1∶0.1,反应温度25℃,反应时间30min。在此条件下,产品1,4-二(2,2’-二吡咯甲基)苯的收率可达85%,纯度可达95%(HPLC)。目标化合物经1HNMR、13CNMR确证。
Using pyrrole and terephthalaldehyde as raw materials, 1,4-bis (2,2’-dipyrromethene) benzene (BDMP) was synthesized in one step using solventless Michael addition reaction. The effects of feed ratio, temperature, catalyst and other factors on the reaction were investigated. The best synthesis conditions are as follows: n (pyrrole): n (terephthalaldehyde): n (propionic acid) = 4:1:1, reaction temperature 25 ℃, reaction time 30min. Under these conditions, the yield of 1,4-bis (2,2’-dipyrromethene) benzene reached 85% with a purity of 95% (HPLC). The target compound was confirmed by 1HNMR, 13CNMR.