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
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摘要: 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,适合工业化生产。Abstract: 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.
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Key words:
- medicinal chemistry /
- process improvement /
- purpurin-18 /
- orthogonal design /
- photosensitizer
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