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Process for the Preparation and Purification of Sodium tetrakis(3,5-bistrifluoromethylphenyl)borate.

IP.com Disclosure Number: IPCOM000012219D
Publication Date: 2003-Apr-17
Document File: 1 page(s) / 63K

Publishing Venue

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Abstract

This invention relates to the development of a new process for the preparation and purification of sodium tetrakis(3,5-bistrifluoromethylphenyl)borate salt, (CAS No. 79060-88-1). This new process leads to increased reaction yields, improved product quality and eliminates the use of halogenated solvents from the material workup. These results were achieved by a modification of the procedure of Brookhart, M. et al, Organometallics, vol. 11, no. 11, 1992, pg. 3920-2). In modified procedure the final extraction with methylene chloride was replaced by successive charcoal treatments in methanol followed by filtration, solvent removal and crystallization to yield the pure product as a light yellow solid with favorable 1H, 13C NMR and melting point data in >85% yield, compared to the literature result of <70% yield.

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Title:  Process for the preparation and purification of Sodium tetrakis(3,5-bistrifluoromethylphenyl)borate.

Abstract:  This invention relates to the development of a new process for the preparation and purification of sodium tetrakis(3,5-bistrifluoromethylphenyl)borate salt, (CAS No. 79060-88-1).  This new process leads to increased reaction yields, improved product quality and eliminates the use of halogenated solvents from the material workup.  These results were achieved by a modification of the procedure of Brookhart, M. et al, Organometallics, vol. 11, no. 11, 1992, pg. 3920-2). In modified procedure the final extraction with methylene chloride was replaced by successive charcoal treatments in methanol followed by filtration, solvent removal and crystallization to yield the pure product  as a light yellow solid with favorable 1H, 13C NMR and melting point data in >85% yield, compared to the literature result of   <70% yield.