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首次以HZSM-5分子筛为催化剂,以间苯二酚和乙酰乙酸乙酯为原料,在无溶剂条件下合成了标题化合物。实验结果表明:HZSM-5分子筛对Pechmann反应有很高的催化活性,具有催化剂用量(0.3 g/0.1 mol间苯二酚)少、产率较高(达96.7%)、后处理简单和无污染、可重复循环利用(循环使用5次产率高达90%以上)等优点。HZSM-5分子筛催化合成标题化合物反应的最佳条件为:V(间苯二酚)∶V(乙酰乙酸乙酯)=1∶1,催化剂用量0.3 g/0.1 mol间苯二酚,反应1.5 h,反应温度约105℃。
For the first time, the title compound was synthesized under the condition of no solvent with HZSM-5 molecular sieve as catalyst and resorcinol and ethyl acetoacetate as raw materials. The experimental results show that the HZSM-5 zeolite has a high catalytic activity for Pechmann reaction, with a small amount of catalyst (0.3 g / 0.1 mol resorcinol), high yield (96.7%), simple post-treatment and no pollution , Can be recycled repeatedly (recycling 5 times the yield of up to 90% or more) and so on. The optimum conditions for the synthesis of the title compound by HZSM-5 zeolite were as follows: V (resorcinol): V (ethyl acetoacetate) = 1: 1, catalyst amount 0.3 g / 0.1 mol resorcinol, reaction 1.5 h , The reaction temperature is about 105 ℃.