乙酸锌催化一步法合成吡咯甲酸甲酯

以乙酸锌为催化剂、碳酸二甲酯(DMC)为甲氧基羰基化试剂,对吡咯一步甲氧基羰基化合成了吡咯甲酸甲酯。实验结果表明,升高反应温度和延长反应时间有利于2-吡咯甲酸甲酯(2-MPC)的生成而不利于1-吡咯甲酸甲酯(1-MPC)的生成,两者的总收率提高,但总选择性降低。采用正交实验对反应的影响因素进行了分析,得到各因素对反应影响程度的大小顺序为:反应温度>反应时间>反应物配比>催化剂用量,其中反应温度和反应时间对反应的影响较为显著。优化的反应条件为:反应温度260℃,反应时间8h,催化剂用量为吡咯质量的5%,DMC与吡咯的摩尔比为4。在此条件下,1-MPC和2-MPC的总收率(相对于吡咯)可达到63.68%。

One-Pot Synthesis of Methyl Pyrrole Carboxylate over Zinc Acetate Catalyst

Methyl pyrrole carboxylates were synthesized via one-pot methoxycarbonylation of pyrrole with dimethyl carbonate(DMC) over zinc acetate catalyst.Increases of both reaction temperature and time favor formation of methyl pyrrole-2-carboxylate(2-MPC) but not methyl pyrrole-1-carboxylate(1-MPC),which might relate to coordination of Zn ion with pyrrole during catalytic process.Higher reaction temperature and longer reaction time increase total yield to 1-MPC and 2-MPC but decrease their total selectivity.Orthogo...