| 引用本文: | 吴爱祥,殷红,张铖,陈思远,王力维,王剑.甲氧苄啶中间体3,4,5-三甲氧基苯甲醛的合成[J].中国现代应用药学,2020,37(13):1584-1589. |
| WU Aixiang,YIN Hong,ZHANG Cheng,CHEN Siyuan,WANG Liwei,WANG Jian.Synthesis of 3,4,5-Trimethoxybenzaldehyde—Intermediate of Trimethoprim[J].Chin J Mod Appl Pharm(中国现代应用药学),2020,37(13):1584-1589. |
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| 甲氧苄啶中间体3,4,5-三甲氧基苯甲醛的合成 |
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吴爱祥1, 殷红2, 张铖2, 陈思远2, 王力维2, 王剑2
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1.宁波大学附属人民医院, 浙江 宁波 315040;2.杭州医学院药学院, 杭州 310000
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| 摘要: |
| 目的 从绿色化学角度出发，得到合成甲氧苄啶中间体3，4，5-三甲氧基苯甲醛（3，4，5-trimethoxybenzaldehyde，TMB）的新工艺。方法 使用溴离子作为溴源，应用氧化溴化等绿色合成方法对合成路线进行优化。结果 在TMB的合成中实现了溴元素的原子经济性利用，与现存工艺相比，避免了溴素的使用，避免了高温、高压反应，总收率达到了77.7%。结论 甲氧苄啶中间体TMB可以通过高原子经济性氧化溴化等多步反应进行合成，收率较高，溴化步骤溴原子利用率可达86.4%。 |
| 关键词: 3,4,5-三甲氧基苯甲醛 合成 氧化溴化 优化 |
| DOI：10.13748/j.cnki.issn1007-7693.2020.13.009 |
| 分类号:R914.5 |
| 基金项目:杭州医学院教学改革重点项目（XJJG2017024）；浙江省高等教育“十三五”第一批教学改革研究项目（jg20180426） |
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| Synthesis of 3,4,5-Trimethoxybenzaldehyde—Intermediate of Trimethoprim |
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WU Aixiang1, YIN Hong2, ZHANG Cheng2, CHEN Siyuan2, WANG Liwei2, WANG Jian2
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1.The Affiliated People's Hospital of Ningbo University, Ningbo 315040, China;2.School of Pharmacy, Hangzhou Medical College, Hangzhou 310000, China
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| Abstract: |
| OBJECTIVE To obtain a new process to synthesize 3,4,5-trimethoxybenzaldehyde(TMB)-intermediate of trimethoprim from the angle of green chemistry. METHODS Synthetic process was optimized with the oxidative bromination and other methods by using bromide ion as a source of bromine. RESULTS In the synthesis of TMB, the economical utilization of bromine was realized. Compared with the existing process, the use of bromine and high temperature and high pressure reactions were avoided, and the total yield reaches 77.7%. CONCLUSION TMB-the intermediate of trimethoprim has been synthesized through high atom-economy oxidative bromination and other steps with decent yields. The yield is high, and the utilization rate of bromine atom in the bromination step can reach 86.4%. |
| Key words: 3,4,5-trimethoxybenzaldehyde synthesis oxidative bromination optimization |
