Method for preparing oltipraz

Details Method for preparing oltipraz Method for preparing oltipraz

2007-10-30

2007-10-30

Tucker, Zachary C (Department: 1624)

Organic compounds -- part of the class 532-570 series

Organic compounds

Nitrogen attached directly or indirectly to the purine ring...

Reexamination Certificate

active

10536492

ABSTRACT:
Provided is a method for preparing oltipraz. The method includes reacting methyl 2-methyl-3-(pyrazin-2-yl)-3oxopropionate with phosphorus pentasulfide in the presence of a mixed solvent of toluene and xylene, followed by recrystallization.

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patent: 2003/0191137 (2003-10-01), Kim et al.
patent: WO 01/09118 (2001-02-01), None
Kugucheva et al, “Gas-Chromatographic Analysis of Trace Impurities for Ethylbenzene, o-, m- and p-xylenes in Toluene” Neftepererabotka i Neftekhimiya, vol. 3, pp. 35-36 (1983). As Abstracted by Caplus.
Iida and Okada “Determination of Trace Impurities in Toluene by Gas Chromatography-Chemical Ionization Mass Spectrometry” Bunseki Kagaku, vol. 26(9), pp. 630-634 (1977). As Abstracted by Caplus.
Hogfeldt, E. “Impurities in Analytical Reagent Grade Chemicals” Journal of Chromatography, vol. 12(1), pp. 112-113 (1963).
Kugucheva et al, “Gas-Chromatographic Analysis of Trace Impurities for Ethylbenzene, o-, m- and p-xylenes in Toluene” Neftepererabotka i Neftekhimiya, vol. 3, pp. 35-36 (1983) Russian-Language Version and English Translation.
Iida and Okada “Determination of Trace Impurities in Toluene by Gas Chromatography-Chemical Ionization Mass Spectrometry” Bunseki Kagaku, vol. 26(9), pp. 630-634 (1977) Japanese-Language Version and English Translation.
Abdaly F., et al., “Synthesis and schistosomicidal activity of 4-methyl-5(aryl vinyl)-1,2-dithiole-3-thiones”,IL Farmaco, 1991, pp. 45-62, vol. 46(1).
Chi W.J., et al., “Oltipraz, a novel inhibitor of hepatitis B virus transcription through elevation of p53 protein”,Carcinogenesis, 1998, pp. 2133-2138, vol. 19(12).
Curphey T.J., “A superior procedure for the conversion of 3-oxoesters to 3H-1,2-dithiole-3-thiones”,Tetrahedron Letters, 2000, pp. 9963-9966, vol. 41.
Curphey T.J., et al., “A new synthesis of 3H-1,2-Dithiole-3-thiones”,Tetrahedron Letters, 1993, pp. 3703-3706, vol. 34(23).
Vaccher C., et al., Preparation and schistosomicidal activity of vinylogues of 1,3-dithio-3-thione,IL Farmaco, 1987, pp. 397-407, vol. 42(6).

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