氮杂环脒类光产碱剂的合成及性能  

Synthesis and Performance of Nitrogen Heterocyclic Amidines as Photobase Generators

作　　者：宋国强[1] 王瑞瑞[1] 李贝贝[1] 冯筱晴[1,2] 

机构地区：[1]常州大学制药与生命科学学院,江苏常州213164 [2]常州市药品制造与质量控制工程重点实验室,江苏常州213164

出　　处：《精细化工》2013年第11期1279-1283,1293,共6页Fine Chemicals

基　　金：江苏省科技成果转化专项资金(BA2012062);常州大学校基金(czuyj10012)~~

摘　　要：以1,5-二氮杂双环[4,3,0]-5-壬烯(DBN)为起始原料,采用氢化铝锂为还原剂,于55℃反应9 h,生成1,5-二氮杂双环[4,3,0]壬烷(Ⅰa),最高收率可达87.9%,色谱纯度大于95.0%。再将Ⅰa分别与4种氯甲基吡啶类化合物反应,合成了系列新型含氮杂环脒类光产碱剂,实验中通过对其工艺条件的考察和优化,得到合成该类光产碱剂最高收率达84.7%,色谱纯度大于95.7%。并对合成的含氮杂环脒类新型光产碱剂进行紫外吸收、感光性、热稳定性等性能测试,分析该系列光产碱剂的构效关系。产品及中间体经高效气相色谱(HPGC)、高效液相色谱(HPLC)、液相色谱-质谱联用(LC-MS)、核磁共振氢谱(1HNMR)对其进行了定量和定性分析。In this paper, 1,5-diazabicyclo [ 4, 3,0 ] nonane was prepared by reduction of 1,5- diazabicyclo [ 4,3,0 ] nonene （DBN） with LiA1H4 in methyl tert-butyl ether at 55 ~C for 9 h. The yield and purity of the product can reach 87.9% and 95% , respectively. This series of amidine photobase generators was synthesized through the reaction of 1,5-diazabicyclo[4,3,0 ] nonane with corresponding chloro-methyl-pyridine compounds and the yield and purity was even up to 84. 7% and 95.7% , respectively. The structure-activity relationship of the photobase-generators was investigated by UV absorbance ,thermal stability and photo-sensitivity and so on. HPLC, LC-MS and I HNMR were also applied to monitor and characterize the intermediates and final products.

关 键 词：DBN 还原 1 5-二氮杂双环[4 3 0]壬烷 光产碱剂 合成工艺 性能研究 精细化工中间体 

分 类 号：TQ314.241[化学工程—高聚物工业]