正交实验设计优化光敏剂紫红素-18的合成工艺

Optimization of the synthesis of photosensitizer purpurin-18 by orthogonal design

目的优化光敏剂紫红素-18（1）的合成工艺。方法以脱镁叶绿酸a（2）为原料,经空气氧化及碱开环制得化合物1;选择影响其合成产率的反应时间（A）、氢氧化钾溶液浓度（B）、反应溶剂（C）和化合物2与氢氧化钾的质量投料比（D）为考察因素,每个因素各取三个水平,采用L9（34）正交试验法优化目标物1的最佳合成工艺。结果合成目标物1的最优反应条件为B1C2A2D2,反应工艺收率从34.4%提高到45.6%。结论新工艺提高了收率、缩短了反应时间、消除了毒性溶剂。

Objective To optimize the synthesis of photosensitizer purpurin-18（1）.Methods Target compound 1 was synthesized through air oxidation and simultaneously ring cleavage of pheophorbide a（2） in presence of alkali.Four main factors influencing synthetic yield of 1 such as reaction time（A）,concentration of potassium hydroxide（B）,solvent（C） and weight ratio of material 2 to potassium hydroxide（D）,which was chosed three levels respectively,were evaluated by the orthogonal experimental design of L9（34）.Results The optimization term of the synthesis of target compound 1 was B1C2A2D2.The yield of 1 was raised from 34.4%to 45.6%.Conclusion The yield was raised.The reaction time was shortened and the toxic solvent was removed. The procedure was suitable for industrial production