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以乙酰乙酸乙酯或丙酰乙酸甲酯(Ⅰ)为起始反应物,在醋酸溶液中发生亚硝化反应可得到相应的肟,肟用锌粉还原为α-胺基羰基化合物后再与1,3-二羰基化合物进行成环缩合反应,合成了5种多吡咯化合物(Ⅳa～Ⅳe)。实验表明,还原和成环缩合的反应条件是影响目标化合物产率的主要因素,该文详细考察了还原和成环缩合反应中锌粉的用量,溶液酸度以及反应温度等条件对产率的影响,确定的最佳反应条件为:n(Zn)∶n(Ⅰ)=(2.7～2.8)∶1.0,pH=4.0～4.5,反应温度95～100℃,在该反应条件下,5种目标化合物的产率可达56%～67%。通过熔点测定、IR和1HNMR等对合成的5种多取代吡咯化合物进行了表征。
Ethyl acetoacetate or propionyl acetate (Ⅰ) as the starting material, nitration in acetic acid solution to give the corresponding oxime, oxime zinc powder reduced to α-aminocarbonyl compound and then with 1 , 3-dicarbonyl compounds were subjected to a ring-closure condensation reaction to synthesize five kinds of polypyrrole compounds (IVa-IVe). The experimental results show that the reaction conditions of reduction and ring condensation are the main factors affecting the yield of the target compound. The effects of the amount of zinc powder, the solution acidity and the reaction temperature on the yield of the reduction and ring-closure condensation were examined in detail. , The optimal reaction conditions were as follows: n (Zn): n (Ⅰ) = (2.7-2.8): 1.0, pH = 4.0-4.5 and reaction temperature 95-100 ℃. Under the reaction conditions, five target compounds The yield can reach 56% ~ 67%. The synthesized five kinds of polysubstituted pyrrole compounds were characterized by melting point determination, IR and 1HNMR.