无溶剂球磨法合成γ-硝基酯化合物  

Synthesis of γ-Nitro Ester Compounds by Solvent-free Ball-milling Method

作　　者：陈达[1] 贾春满[1] 张春艳[1] 张岐[1] 曹丽[1] 孙璐[1] 梁利邦 

机构地区：[1]海南大学海南省精细化工重点实验室,海南海口570228

出　　处：《精细化工》2014年第1期124-128,共5页Fine Chemicals

基　　金：国家自然科学基金(21166008;21261008);海南自然科学基金(213014);海南大学青年基金(qnjj1169)~~

摘　　要：采用球磨法在无溶剂条件下用硝酸钙促进硝基烯烃与丙二酸酯发生迈克尔加成反应,从而合成γ-硝基酯化合物。该反应在频率为20 Hz下进行,30 min即可完全转化。硝基烯烃及其衍生物与丙二酸酯反应可得到产率80%以上的目标产物,尤其当硝基苯乙烯苯环上的邻位有两个吸电子基时,产率可达95%。A calcium nitrate prompted solvent-free Michael addition reaction of nitroalkenes with malonate esters to synthesize γ-nitro ester compounds by ball-milling method has been developed. The reaction was carried out at a frequency of 20 Hz, and took 30 min to complete the conversion. Nitroalkenes and their derivatives reacted with malonate esters to obtain the target product with a yield of more than 80%. Especially,when there were two electron-withdrawing groups in the ortho position of the phenyl ring of nitrostyrene, the yield was up to 95 %.

关 键 词：球磨法 绿色化学 γ-硝基酯 迈克尔加成 精细化工中间体 

分 类 号：TQ246.12[化学工程—有机化工] TQ021.5