Method for the preparation of the monopotassium salt of 1,...

C - Chemistry – Metallurgy – 07 – D

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260/308.3

C07D 285/10 (2006.01)

Patent

CA 1083580

ABSTRACT OF THE DISCLOSURE : Process for the preparation of the monopotassium salt of 1,2,5-thiadiazol-3,4-dicarboxylic acid (I). Involves double-stage saponification of 3,4-dicyano-1,2,5-thiadiazole (II), 3-cyano-4-carboamoyl-1,2,5-thiadiazole (III) is obtained from an aqueous suspension of 3,4-dicyano-1,2,5-thiadiazole (II) by catalytic hydration through the addition of aqueous KOH, desirably at a temperature of from 20° to 50°C. and with a molar ratio of 3,4-dicyano-1,25-thiadiazole (II) to KOH of from 1:0.01 and 1:0.8. This is followed by hydrolysis, by the further addition of aqueous KOH, desirably at a temperature of from 85 to 100°C, until attaining an overall molar ratio of 3,4-dicyano-1,2,5-thiadiazole (II) to KOH of from about 1:2.0 and 1:2.35, a molar ratio of 3,4-dicyano-1,2,5-thiadiazole (II) to H20 of from about 1:20 to 1:23. Thereafter, from the resulting solution of dipotassium salt of 1,2,5-thiadiazole- 3,4-diccarboxylic acid, the monopotassium salt is separated by acidification of said solution.

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