Sulfuric Acid → 2,4-Di-tert-butyl-6-{4-[3-(4,5-dimethyl-4h-[1,2,4]triazol-3-ylsulfanyl)-propyl]-piperazin-1-yl}-pyrimidine mono-sulfate salt

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Reaction Steps

2,4-Di-tert-butyl-6-{4-[3-(4,5-dimethyl-4H-[1,2,4]triazol-3-ylsulfanyl)-propyl]-piperazin-1-yl}-pyrimidine (1.0 g, 2.2 mmol) was dissolved in isopropanol at 60° C. A solution of concentrated sulfuric acid (0.22 g, 98%, 2.2 mmol) in isopropanol (1 mL) was added giving a clear solution. Ethyl acetate (20 mL) was slowly added keeping the flask at ˜50° C. The resulting slurry was cooled to ambient temperature and stirred overnight. The precipitate was filtered, rinsed with 10 mL ethyl acetate and vacuum dried at 40° C. overnight to give 2,4-Di-tert-butyl-6-{4-[3-(4,5-dimethyl-4H-[1,2,4]triazol-3-ylsulfanyl)-propyl]-piperazin-1-yl}-pyrimidine mono-sulfate salt (1.06 g). Yield: 86.9%.

Provenance & Evidence