摘要
以(E)-2,4-二硝基二苯乙烯类化合物为原料,利用分子筛催化一步合成7个(E)-α,2,4-三硝基二苯乙烯类化合物。考察硝化体系、催化剂种类、反应温度及反应时间等因素对整个反应的影响,并进一步优化工艺条件。结果表明:较优的工艺条件为丙酸酐15.0 m L,10倍当量的硝酸,0.20 g Hβ分子筛(n(Si)/n(Al)=300),室温下反应5~10 min,硝化产物产率能达到85%以上。该方法反应条件温和,具有较高的选择性和通用性。为进一步确定该类化合物产物结构,通过X线单晶衍射对产物7的结构进行了分析。
Seven( E)-α,2,4-trinitrostilbenes catalyzed by zeolites in one step were afforded with( E)-2,4-dinitrostilbenes as starting materials.The effects of nitration systems,catalyst types,reaction temperatures and time were investigated,and the process parameters were optimized. The reaction conditions were optimized as follows: propionic anhydride of 15. 0 m L,nitric acid of 10 equiv,Hβ zeolite( n( Si)/n( Al)= 300) of 0. 20 g,reaction time of 5 ~ 10 min at room temperature,the yield of nitrated product was more than 85%. This method were used in very mild conditions with high compatibility and selectively. To confirm the product structures,the compound 7 was unequivocally proven by single crystal X-ray diffraction.
引文
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