| 正交设计优化光敏剂二氢卟吩e6-C15单甲酯的合成工艺 |
| 投稿时间：2014-08-26 修订日期：2014-11-17 点此下载全文 |
| 引用本文：单彬,孙渺,孟志,韩贵焱,钱其涵,刘明辉,姚建忠.正交设计优化光敏剂二氢卟吩e6-C15单甲酯的合成工艺[J].药学实践杂志,2015,33(2):122~124 |
| 摘要点击次数: 1023 |
| 全文下载次数: 318 |
|
| 基金项目:国家自然科学基金(81172950);上海市科委重点科技攻关项目(11431920401) |
|
| 中文摘要:目的 优化光敏剂二氢卟吩e6-C15单甲酯 (1)的合成工艺。 方法 采用"一锅法", 以脱镁叶绿酸a 为原料, 通N2条件下经碱甲醇液作用下E环开裂后直接添加1/20体积量的水, 回流水解制得化合物1。选择影响其合成产率的开环反应时间(A)、回流水解反应时间(B)、氢氧化钾甲醇液浓度(C)、3与氢氧化钾的质量投料比(D)为主要考察因素, 每个因素各取3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 合成化合物1的最优反应条件为B1C2A2D1, 工艺收率从43.0%提高到56.5%。结论该工艺具有操作简便、安全、收率高等优点, 适合工业化生产。 |
| 中文关键词:工艺改进 二氢卟吩e6-C15单甲酯 正交设计 光敏剂 |
| |
| Optimization of synthesis of photosensitizer chlorin e6-C15 monomethyl ester by the orthogonal design |
|
|
| Abstract:Objective To optimize the synthesis of photosensitizer chlorine e6-C15 monomethyl ester (1). Methods Target compound 1 was synthesized through E ring cracking of pheophorbide a (3) in methanol solution of potassium hydroxide followed by adding H2O for ester hydrolysis with "one-pot" process. Four main factors that influencing the synthetic yield of target compound 1 are ring cleavage reaction time (A), reflux hydrolysis reaction time (B), alkali concentration (C) and weight ratio of material 3 to alkali (D). Each of the four factors was chosen at three levels and evaluated by the orthogonal experimental design of L9 (34). Results The optimization terms of the synthesis of target compound 1 were B1C2A2D1. The yield of compound 1 was raised from 43.0% to 56.5%. Conclusion The developed process has the advantages of simple operation, good safety and high reaction yield, and is suitable for industrial production. |
| keywords:process improvement chlorine e6-C15 monomethyl ester orthogonal design photosensitizer |
| 查看全文 查看/发表评论 下载PDF阅读器 |
|
| 关闭 |
|
|
|
