| STAT3抑制剂（HO-3867）的合成工艺改进 |
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| 引用本文： | 苏进财,翁智兵,周国春.STAT3抑制剂（HO-3867）的合成工艺改进[J].合成化学,2016,24(2):155-159. |
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| 作者姓名： | 苏进财 翁智兵 周国春 |
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| 作者单位： | 南京工业大学 药学院，江苏 南京 211816 |
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| 基金项目： | 国家自然科学基金资助项目(30973621) |
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| 摘 要： | 以3,5-二溴-2,2,6,6-四甲基-4-哌啶酮为起始原料，经Favorskii重排和氧化反应的一锅法制得甲基-1-氧基-2,2,5,5-四甲基吡咯烷-3-羧酸甲酯(5a)；低温下用四氢铝锂还原5a制得3-羟甲基-1-氧基-2,2,5,5-四甲基吡咯啉(7)； 7溴化后与芳胺发生烷基化反应，半连续合成了STAT3抑制剂（HO-3867）,总产率46.3%,其结构经1H NMR和HR-ESI-MS确证。
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| 关 键 词： | HO-3867 一锅法合成 半连续合成 药物合成 工艺改进 |
| 收稿时间： | 2015-08-31 |
Process Improvement on Synthesis of STAT3 Inhibitor (HO-3867) |
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| SU Jin-cai,WENG Zhi-bing,ZHOU Guo-chun.Process Improvement on Synthesis of STAT3 Inhibitor (HO-3867)[J].Chinese Journal of Synthetic Chemistry,2016,24(2):155-159. |
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| Authors: | SU Jin-cai WENG Zhi-bing ZHOU Guo-chun |
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| Institution: | School of Pharmaceutical Sciences, Nanjing Tech University, Nanjing 211816, China |
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| Abstract: | Methyl 1-oxyl-2,2,5,5-tetramethylpyrroline-3-carboxylate(5a) was prepared by one-pot method of Favorskii reaction and oxidation, using 3,5-dibromo-2,2,6,6-tetramethylpiperidin-4-one as starting material. 3-Hydroxymethyl-1-oxy-2,2,5,5-tetramethyl pyrroline(7) was obtained by low temperature reduction reaction of 5a, using LiAlH4 as reducing agent. HO-3867 was synthesized by semi-continuous method of alkylation reaction of brominized 7 with arylamine. The total yield was 46.3%. The structure was confirmed by 1H NMR and HR-ESI-MS. |
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| Keywords: | HO-3867 one-pot synthesis semi-continuous synthesis drug synthesis process improvement |
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