Removal of Palladium from Organic Reaction Mixtures by Trimercaptotriazine

Autor: Rosso, V. W., Lust, D. A., Bernot, P. J., Grosso, J. A., Modi, S. P., Rusowicz, A., Sedergran, T. C., Simpson, J. H., Srivastava, S. K., Humora, M. J., Anderson, N. G.
Zdroj: Organic Process Research & Development; July 1997, Vol. 1 Issue: 4 p311-314, 4p
Abstrakt: 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.
Databáze: Supplemental Index