| 程纯儒,丁杰,杨义,柯鸿.化学通报,2014,77(5):467-470. |
| 间叔丁基苯乙醚的合成研究 |
| The Synthesis of 1-Tert-butyl-3-ethoxybenzene |
| 投稿时间：2014-01-11 修订日期：2014-01-19 |
| DOI： |
| 中文关键词: 间叔丁基苯乙醚 乙螨唑 有机中间体合成 对叔丁基苯乙醚 |
| 英文关键词:1-Tert-butyl-3-ethoxybenzene, Etoxazole, Organic intermediate, 1-Tert-butyl-4-ethoxybenzene |
| 基金项目: |
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| 摘要点击次数: 4275 |
| 全文下载次数: 3 |
| 中文摘要: |
| 本文分别采用叔丁基苯和对氨基叔丁基苯为原料,通过两条新的合成路线合成了生产新型农药乙螨唑的关键中间体间叔丁基苯乙醚。合成路线一以叔丁基苯为原料,通过溴代、硝化、还原(脱卤素)、重氮化和乙醚化反应得到目标化合物间叔丁基苯乙醚；合成路线二采用对氨基叔丁基苯为原料,通过乙酰化、溴代、脱乙酰化、重氮化去氨基和乙醚化反应得到目标化合物间叔丁基苯乙醚。两条合成路线的总收率较高,分别为45%和63%。所得产品中未检测到异构体对叔丁基苯乙醚,质量好,纯度高。其中合成路线一原料便宜,操作简单,更适合进一步工业化放大生产。合成路线中的有机中间体和目标化合物的化学结构通过MS和NMR数据进行确证。其中,目标化合物间叔丁基苯乙醚的波谱数据为首次报道。 |
| 英文摘要: |
| 1-Tert-butyl-3-ethoxybenzene, which is an important organic intermediate for the production of Etoxazole, was synthesized through two synthetical routes using tert-butylbenzene and 4-tert-butylbenzenamine as the starting material, respectively. In synthetic route one, 1-tert-butyl-3-ethoxybenzene was synthesized from tert-butylbenzene via bromination, nitration, reduction (dehalogenation), diazotization and ethanolysis; In synthetic route two, 1-tert-butyl-3-ethoxybenzene was synthesized from 4-tert-butylbenzenamine via acylation, bromination, deacylation, diazotization and ethanolysis. The total yields were 45% and 63%, respectively. The purity of the final produt was high, no isomer (1-tert-butyl-4-ethoxybenzene) was detected. The starting material of synthetical route one is cheaper, and the procedure of synthetical route one is simple. Herein, synthetical route one was more appropriate for the industrialization. The structures of the intermediate and the target compound were confirmed by MS and NMR. The spectroscopic data of the final compound was reported for the first time. |
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