三巯基三嗪去除有机反应混合物中的钯

IF 3.5 3区化学 Q2 CHEMISTRY, APPLIED

Organic Process Research & Development Pub Date : 1997-07-15 DOI:10.1021/op970107f

Victor W. Rosso, David A. Lust, Peter J. Bernot, John A. Grosso, Sandeep P. Modi, Andrew Rusowicz, Thomas C. Sedergran, James H. Simpson, Sushil K. Srivastava, Michael J. Humora, Neal G. Anderson

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引用次数: 89

摘要

在努力去除残留的钯从候选药物制备的钯催化吲哚，许多治疗方法进行了研究。最有效的处理方法是使用2,4,6-三巯基-s-三嗪(TMT)从溶液中沉淀钯，这将钯的含量从600?650 PPM到20 PPM ?60 PPM的分离吲哚中间体。随后的结晶通常提供含有1ppm钯的活性药物成分。TMT处理应证明对降低其他反应中残余钯的浓度是有用的。

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Removal of Palladium from Organic Reaction Mixtures by Trimercaptotriazine

In an effort to remove residual palladium from a drug candidate prepared by palladium-catalyzed indolization, many treatments were examined. The most effective treatment was to precipitate palladium from solution using 2,4,6-trimercapto-s-triazine (TMT), which reduced palladium levels from 600?650 ppm to 20?60 ppm in an isolated indole intermediate. Subsequent crystallizations routinely afforded active pharmaceutical ingredient with <1 ppm of palladium. TMT treatment should prove useful to reduce the concentration of residual palladium in other reactions.

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来源期刊

Organic Process Research & Development 化学-应用化学

CiteScore

6.90

自引率

14.70%

发文量

251

审稿时长

2 months

期刊介绍： The journal Organic Process Research & Development serves as a communication tool between industrial chemists and chemists working in universities and research institutes. As such, it reports original work from the broad field of industrial process chemistry but also presents academic results that are relevant, or potentially relevant, to industrial applications. Process chemistry is the science that enables the safe, environmentally benign and ultimately economical manufacturing of organic compounds that are required in larger amounts to help address the needs of society. Consequently, the Journal encompasses every aspect of organic chemistry, including all aspects of catalysis, synthetic methodology development and synthetic strategy exploration, but also includes aspects from analytical and solid-state chemistry and chemical engineering, such as work-up tools，process safety, or flow-chemistry. The goal of development and optimization of chemical reactions and processes is their transfer to a larger scale; original work describing such studies and the actual implementation on scale is highly relevant to the journal. However, studies on new developments from either industry, research institutes or academia that have not yet been demonstrated on scale, but where an industrial utility can be expected and where the study has addressed important prerequisites for a scale-up and has given confidence into the reliability and practicality of the chemistry, also serve the mission of OPR&D as a communication tool between the different contributors to the field.