Real-Time Monitoring of Solid-Liquid Slurries: Optimized Synthesis of Tetrabenazine
Solid-liquid slurries are vital and increasingly prevalent in the pharmaceutical and chemical industries. Despite the importance of these heterogeneous systems, process control and optimization are fundamentally hindered by a lack of compatible real-time analytical techniques. We present herein an online HPLC monitoring platform enabling access to real-time compositional information on slurries. We demonstrate the system by investigating the heterogeneous synthesis reaction of tetrabenazine. Furthermore, we integrated our online HPLC platform with the orthogonal monitoring techniques of a pH probe and a microscopic imaging probe to provide additional mechanistic insight. These combined insights enable the optimization of tetrabenazine synthesis in terms of reaction time, byproduct formation, and diastereomeric purity of the final product.
Sato, Yusuke,Liu, Junliang,Kukor, Andrew J.,Culhane, Jeffrey C.,Tucker, John L.,Kucera, David J.,Cochran, Brian M.,Hein, Jason E.
p. 14069 - 14078
(2021/07/26)
β-Silylcarbonyl Compounds as Masked Enones
β-Trimethylsilylketones and lactones can be brominated (3)->(4) and desilylbrominated (4)->(5) specifically to place a double bond between the carbonyl group and the β-carbon atom to which the silicon had originally been bound.The silyl group therefore is a base- and acid stable group masking the α,β-unsaturation of enones.Several α-methylene-ketones and -lactones have been prepared in this way.With ketones, the bromination step seems always to introduce bromine mainly or exclusively at the α-position on that side of the ketone on which the β-silyl group is placed, regardless of whether it is more or the less substituted α-position.
Fleming, Ian,Goldhill, Jon
p. 1493 - 1498
(2007/10/02)
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