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作 者:刘万兴 曹翠莲 王凯 路玉坤 刘秀峥 LIU Wan-xing;CAO Cui-lian;WANG Kai;LU Yu-hun;LIU Xiu-zheng(The Non-public Enterprise Service Center of Liaocheng,Liaocheng 252000,China;The Key Laboratory of Research on Green Adhesive System for Tire with Aramid as Skeleton Material of Liaocheng,Liaocheng 252000,China;Liaocheng Kinge Synthetic Material Co.,Ltd.,Liaocheng 252000,China)
机构地区:[1]聊城市非公有制企业服务中心,山东聊城252000 [2]聊城市以芳纶为骨架材料的轮胎用绿色粘合体系研究重点实验室,山东聊城252000 [3]聊城金歌合成材料有限公司,山东聊城252000
出 处:《精细化工中间体》2023年第5期37-41,共5页Fine Chemical Intermediates
摘 要:以4-溴苯乙腈和1,1-二(甲硫基)-2-硝基乙烯为原料,二甲基亚砜为溶剂,经过4步反应,获得3-(4-溴苯基)吡咯烷-2,5-二酮。反应时间为24、2、48、3.5 h时,收率分别为75.2%、76.8%、77.8%、78.5%,纯度分别为95.6%、96.6%、97.5%、97.8%(HPLC)。对终产物和标准样对比测定熔点、~1H NMR进行表征。Using 4-bromophenylacetonitrile and 1,1-bis(methylthio)-2-nitroethylene as raw materials and Dimethyl sulfoxide as solvent,the final product 3-(4-bromophenyl)pyrrolidine-2,5-dione was obtained in a 4-step reaction.The reaction time was 24,2,48 and 3.5 h respectively,and the yields were 75.2%,76.8%,77.8%and 78.5%respectively.The final product was characterized by'H NMR.Compared with the standard sample,the softening point was determined,and the purity was 95.6%,96.6%,97.5%and 97.8%by HPLC.
关 键 词:4-溴苯乙腈 1 1-二(甲硫基)-2-硝基乙烯 3-(4-溴苯基)吡咯烷-2 5-二酮 合成 核磁
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