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
-
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.
-
Key words:
- medicinal chemistry /
- process improvement /
- purpurin-18 /
- orthogonal design /
- photosensitizer
-
[1] 袁 媛,周传农.光动力治疗诱导肿瘤细胞凋亡的分子作用机制[J].中国激光医学杂志,1996, 5(2): 111. [2] 沈卫镝,姚建忠,方 勇,等. 叶绿素a降解产物紫红素-18的光动力效应[J].中国医药工业杂志,2001, 32(5): 217. [3] 姚建忠,许德余,陈文晖,等. 蚕沙叶绿素的降解及二氢卟吩P6酰胺衍生物的合成[J].中国医药工业杂志,1999, 30(9): 403. [4] 周怀梧. 医药用数理统计[M]. 济南:山东教育出版社,1986:148. [5] 张春华,严云良. 医药用数理统计[M]. 北京:科学出版社,2001:205. -
点击查看大图
计量
- 文章访问数: 3405
- HTML全文浏览量: 251
- PDF下载量: 110
- 被引次数: 0
下载:
