氦杂环脒类光产碱剂的合成及性能
Synthesis and Performance of Nitrogen Heterocyclic Amidines as Photobase Generators
宋国强 1王瑞瑞 1李贝贝 1冯筱晴2
作者信息
- 1. 常州大学制药与生命科学学院,江苏常州213164
- 2. 常州大学制药与生命科学学院,江苏常州213164;常州市药品制造与质量控制工程重点实验室,江苏常州213164
- 折叠
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9h,生成1,5-二氮杂双环[4,3,0]壬烷(Ⅰ a),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.
Abstract
In this paper,1,5-diazabicyclo [4,3,0] nonane was prepared by reduction of 1,5-diazabicyclo[4,3,0] nonene(DBN) with LiAlH4 in methyl tert-butyl ether at 55 ℃ 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 1HNMR 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Key words
DBN/reduction/1,5-diazabicyclo [4,3,0] nonane/photolatent base/synthesis process/performance/fine chemical intermediates引用本文复制引用
基金项目
江苏省科技成果转化专项资金(BA2012062)
常州大学校基金(czuyj10012)
出版年
2013
NETL
NSTL
万方数据