脱氢枞基咪唑啉的制备及结构表征  

Preparation and Structure Identification of Dehydroabietyl Imidazoline

作　　者：蒋少芳 黄道战[1] 蓝虹云[1] 伍岳南 杨伟鹏[1] 

机构地区：[1]广西民族大学化学化工学院广西林产化学与工程重点实验室,广西南宁530008

出　　处：《精细化工》2015年第5期587-591,共5页Fine Chemicals

基　　金：国家自然科学基金(31460174);广西科学研究与技术开发计划项目(1348006-10);广西民族大学引进人才科研启动项目(2014MDQD014)~~

摘　　要：对脱氢枞酸二乙烯三胺盐(Ⅱ)进行热重分析,提出了一种制备脱氢枞基咪唑啉(Ⅳ)的方法。将脱氢枞酸(Ⅰ)用带水剂二甲苯溶解,滴加到热的二乙烯三胺(DETA)中进行高温液液短接触脱水缩合反应,得到产品;DETA既是反应物,又是产品的不良溶剂,还起到调控反应温度的作用;二甲苯受热快速蒸发并将反应生成的水带离反应体系。反应结束后,该产品易于从反应混合物中冷却结晶析出、过滤分离,经元素分析、红外光谱、紫外光谱、1HNMR及13CNMR核磁共振谱的波谱结构表征确证。反应物料比可以改变反应体系的温度,进而对产品产率与外观色泽有较大的影响;在化合物Ⅰ的用量为30 mmol、DETA与化合物Ⅰ的物质的量之比为15.7、反应温度为210℃的条件下,产品产率为86.0%。Based on analyses of the thermogravimetric curve TG/DTG of dehydroabietic acid diethylenetriamine salt （ Ⅱ ） , a method for preparation of dehydroabietyl imidazoline （ Ⅳ ） has been developed. A solution of dehydroabietic acid （ Ⅰ ） in xylene used as water-carrying agent was dropwise added to the hot diethylenetriamine （DETA） to give the product via a high temperature liquid-liquid- short-contact dehydration condensation reaction. The product has a poor solubility in DETA, which is usd as the reactant and can regulate reaction temperature; the water produced by dehydration condensation was easily taken out of the reaction system by xylene, which was fast heated and evaporated. The product was easily separated from reaction mixtures via cool crystallization, and structurally identified by means of EA, IR, UV,1HNMR and 13CNMR. Molar ratio of DETA to compound I could change the reaction temperature, which has obvious effect on the yield and color of the product. Under the reaction conditions （ amount of compound Ⅰ ,30 m mol ; molar ratio of DATE to compound Ⅰ ,15.7 ：reaction temperature.210 ℃ ：reaction time,4 h） ,the yield is 86.0%.

关 键 词：脱氢枞基咪唑啉 脱氢枞酸 二乙烯三胺 脱水缩合 高温液液短接触反应 精细化工中间体 

分 类 号：TQ351[化学工程]