Development of a catalytic tributyltin hydride cyclisation process
Development of a catalytic tributyltin hydride cyclisation process
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DOI：
10.1021/op9900941
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发表时间：
2000-03-01
影响因子：
3.4
通讯作者：
Wanders, A
中科院分区：
文献类型：
--
作者：
Attrill, RP;Blower, MA;Wanders, A
描述了通过自由基环化反应由四氢吡啶 (4) 制备螺环哌啶 (2) 的中试工厂工艺的开发。该中试工厂工艺涉及使用催化量的氢化三丁基锡（0.14当量），该氢化三丁基锡是通过氯化三丁基锡与硼氢化钠（1.1当量）在含有偶氮二异丁腈（AIBN）的2-丙醇/乙醇中反应而就地生成的。描述了最初的实验室条件以及转移到中试工厂时所做的变化。报告了所生产的批次(2)中锡残留量水平的测量结果。
The development of a pilot plant process to prepare the spirocyclic piperidine (2) from the tetrahydropyridine (4) via a radical cyclisation reaction is described. The pilot plant process involves the use of a catalytic amount of tributyltin hydride (0.14 equiv) generated in situ by the reaction of tributyltin chloride with sodium borohydride (1.1 equiv) in 2-propanol/ethanol containing azo-bis(isobutyronitrile) (AIBN). Initial laboratory conditions are described as well as the changes made on transfer to the pilot plant. Measurement of the levels of residual amounts of tin in the batches of (2) produced are reported.