Development of a Catalytic Tributyltin Hydride Cyclisation Process
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- 作者：Robin P. Attrill ; Mark A. Blower ; Keith R. Mulholland ; John K. Roberts ; John E. Richardson ; Martin J. Teasdale ; and Andre Wanders
- 刊名：Organic Process Research & Development
- 出版年：2000
- 出版时间：March 2000
- 年：2000
- 卷：4
- 期：2
- 页码：98 - 101
- 全文大小：56K
- 年卷期：v.4,no.2(March 2000)
- ISSN：1520-586X
文摘
The development of a pilot plant process to prepare thespirocyclic piperidine (2) from the tetrahydropyridine (4) viaa radical cyclisation reaction is described. The pilot plantprocess involves the use of a catalytic amount of tributyltinhydride (0.14 equiv) generated in situ by the reaction oftributyltin chloride with sodium borohydride (1.1 equiv) in2-propanol/ethanol containing azo-bis(isobutyronitrile) (AIBN).Initial laboratory conditions are described as well as the changesmade on transfer to the pilot plant. Measurement of the levelsof residual amounts of tin in the batches of (2) produced arereported.