摘要
目前有关荧烷染料中间体的合成方法国内少有报道。2-羟基-4-(N-乙基-N-异丁基)氨基-2’-羧基二苯酮是一种重要的荧烷类压热敏染料中间体,本文以N-乙基-N-异丁基间氨基苯酚为原料与邻苯二甲酸酐在氮气保护下反应合成,并在反应后使用NaOH溶液分解副产物,以提高产物纯度,通过HPCE测定产物纯度达到96.36%(面积归一法)。使用TLC对反应进程进行监测,并通过UV对TLC检测结果进行确认,详细讨论了物料比、温度和时间等条件对反应的影响,并得出二苯酮合成反应中N-乙基-N-异丁基间氨基苯酚与邻苯二甲酸酐摩尔比为1∶1.5,温度为110℃,时间为15h时反应效果最佳。副产物若丹明染料分解反应中NaOH溶液浓度为33.3%,N-乙基-N-异丁基间氨基苯酚与NaOH的质量比为1∶7.5,温度为90℃,时间为9h时反应效果最佳。最后通过IR和UV对目标产物结构进行确认。
There are few reports about the synthesis of fluorane intermediate in China. 2- hydroxybenzoyl-4-（N-ethyl-N-isobutyl） amino-2＇ -carboxyl benzophenone is a very important intermediate of fluorane thermal-pressure sensitive dyes, it was synthesized with N-ethyl-N- isobutyl-m-aminophenol m-aminophenol and phthalic anhydride. After the synthesis reaction we used NaOH solution to purify the product. HPCE was used to detect the purity of 2- hydroxybenzoyl-4-（N-ethyl-N-isobutyl） amino-2 ＇-carboxyl benzophenone and the purity achieves 96.36% （area normalization method）. TLC was used to monitor the reaction process and we used UV to confirm the conclusion of TLC, the effect of material ratio, temperature and time were discussed in detail, we concluded that in the synthetic reaction of benzophenone, the best reaction condition was the mole ratio of N-ethyl-N-isobutyl-m-aminophenol m-aminophenol and phthalic anhydride was 1 ： 1.5, temperature was 110℃, time was 15h. In the decomposition reaction of by-products, the best reaction condition was the concentration of NaOH solution was 33. 3%, the mass ratio of N-ethyl-N-isobutyl-m-aminophenol m-aminophenol and NaOH was 1 ： 7. 5, temperature was 90℃, time was 9h. At last the target product was confirmed by IR and UV.
出处
《化工进展》
EI
CAS
CSCD
北大核心
2016年第B11期335-339,共5页
Chemical Industry and Engineering Progress
基金
辽宁省教育厅科研项目(LS 2010119)
