Development of a Safe and Robust Process for the Large-Scale Preparation of a Vinyl Bromide from a Ketone Using a (PhO)3P/Br2-Derived Reagent
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- 作者：Nachiket Likhite ; Sivaraj Ramasamy ; Shankar Tendulkar ; Shunmugaraj Sathasivam ; Michael Luzung ; Ye Zhu ; Neil Strotman ; Jeffrey Nye ; Adrian Ortiz ; Susanne Kiau ; Martin D. Eastgate ; Rajappa Vaidyanathan
- 刊名：Organic Process Research & Development
- 出版年：2016
- 出版时间：May 20, 2016
- 年：2016
- 卷：20
- 期：5
- 页码：977-981
- 全文大小：317K
- 年卷期：0
- ISSN：1520-586X
文摘
The large-scale synthesis of ethyl 4-bromocyclohex-3-enecarboxyalate, using a mild brominating reagent derived from triphenyl phosphite and bromine, is reported. The development and comparison of both continuous and batch processes are described. A modified addition sequence was developed based on the knowledge garnered from flow-processing, resulting in a safe and efficient process for the in situ generation of the unstable active reagent and its immediate reaction with the ketone in a batch mode process.