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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。
Using 1,5-diazabicyclo [4,3,0] -5-nonene (DBN) as starting material and lithium aluminum hydride as reducing agent, the reaction was carried out at 55 ℃ for 9 h to produce 1,5-bis Azabicyclo [4,3,0] nonane (Ⅰa), the highest yield of 87.9%, chromatographic purity of more than 95.0%. Then Ia and four kinds of chloromethyl pyridine compounds were synthesized, and a series of novel nitrogen-containing heterocyclic amidine photobase generators were synthesized. Through the investigation and optimization of the process conditions, the synthesis of such photobase generators The highest yield of 84.7%, chromatographic purity greater than 95.7%. The new type of photobase generator containing nitrogen-containing heterocyclic amines was tested for its UV absorption, photosensitivity and thermal stability. The structure-activity relationship of this series of photobase generators was analyzed. The products and intermediates were quantitatively and qualitatively analyzed by high performance gas chromatography (HPGC), high performance liquid chromatography (HPLC), liquid chromatography-mass spectrometry (LC-MS) and 1H nuclear magnetic resonance (1HNMR).