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球磨条件下无溶剂法合成诺卜酮的研究:反应参数的研究。

An alternative solvent-free synthesis of nopinone under ball-milling conditions: Investigation of reaction parameters.

机构信息

Institute for Technical Chemistry and Environmental Chemistry, Friedrich-Schiller University Jena, Lessingstraße 12, 07743 Jena, Germany.

出版信息

ChemSusChem. 2010 Oct 25;3(10):1181-91. doi: 10.1002/cssc.201000122.

DOI:10.1002/cssc.201000122
PMID:20737534
Abstract

A new method for the oxidative cleavage of β-pinene (1) yielding nopinone (2) with potassium permanganate as oxidant under solvent-free conditions was established. The reaction was performed in a conventional ball mill with use of a grinding auxiliary. The auxiliary has the ability to sorb liquid reactants such as 1 on its surface to make liquid(s) accessible for mechanical impact. Different reaction parameters and technical variables were assessed concerning their influence on yield and selectivity of 2. Different chemical parameters such as oxidants, grinding auxiliaries, and quantities were investigated. Also tuning parameters including milling time, rotation frequency, and number of milling balls were explored.

摘要

建立了一种在无溶剂条件下,以高锰酸钾为氧化剂,将β-蒎烯(1)氧化裂解生成诺蒎酮(2)的新方法。该反应在常规球磨机中进行,使用研磨助剂。该助剂具有在其表面吸附 1 等液体反应物的能力,使液体能够受到机械冲击。评估了不同的反应参数和技术变量对 2 的产率和选择性的影响。研究了不同的化学参数,如氧化剂、研磨助剂和用量。还探索了包括研磨时间、旋转频率和研磨球数量在内的调整参数。

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