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合成N,N’-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰]六甲撑二胺的新工艺
引用本文:吕九琢,李燕芸,刘霞,袁光,刘文涛,李润波,冯飞. 合成N,N’-双[3-(3,5-二叔丁基-4-羟基苯基)丙酰]六甲撑二胺的新工艺[J]. 精细化工, 1999, 16(3): 29-32
作者姓名:吕九琢  李燕芸  刘霞  袁光  刘文涛  李润波  冯飞
作者单位:北京石油化工学院,化工系,北京,102600
摘    要:以3 (3,5 二叔丁基 4 羟基苯基)丙酸甲酯(简称3,5 甲酯)与己二胺为原料,甲苯为溶剂,在二正辛基氧化锡(简称有机锡)催化下合成了题示化合物。考察了催化剂、反应温度、反应时间和物料配比等影响因素,得到的优化反应条件为:3,5 甲酯与己二胺摩尔比为(2.1~2.2)∶1,反应温度为110~130℃,反应时间为5h,有机锡用量为3,5 甲酯质量的2%,收率稳定在96%以上。粗产品经一次重结晶后透光率为99%(500nm)和98%(425nm)。提出了反应机理,用元素分析、红外光谱、核磁共振对产品进行了确证。

关 键 词:抗氧剂;氨解反应;3-(3.5-二叔丁基-4-羟基苯基)丙酸甲酯

Synthesis of N,N'-Bis-[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl]-hyxamethylene-diamine by a New Method
Lü Jiu-zhuo,LI Yan-yun,LIU Xia,YUAN Guang,LIU Wen-tao,LI Run-bo,FENG Fei. Synthesis of N,N'-Bis-[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionyl]-hyxamethylene-diamine by a New Method[J]. Fine Chemicals, 1999, 16(3): 29-32
Authors:Lü Jiu-zhuo  LI Yan-yun  LIU Xia  YUAN Guang  LIU Wen-tao  LI Run-bo  FENG Fei
Abstract:The title compound was synthesized in the solvent of toluene with methyl3(3,5ditertbutyl4hydroxyphenyl)propionate() and hexamethylenediamine()as raw materials, organictin as catalyst.The catalyst agent,temperature of the reaction,time of the reaction and the ratio of the raw materials were inspected.The optimum technological conditions were determined that the reaction took place at 110130 for 5h with 2% organictin (based the mass of ) and the molar ratio of /=(2.12.2)/1.Excellent yield (96%) and transmittance (500nm:99%;425nm:98%)were obtained. The reaction mechanism was proposed and the product was characterized by elementary analysis,IR,1HNMR.=
Keywords:antioxidant  ammoniating reaction  methyl(3  5ditertbutyl4hydroxyphenyl)propionate=  
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