2-Methyl-2-thiopseudourea sulfate → HCID 13088591, compound

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Reaction Steps

289 g (1 mol) of 1-(4-chlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)-pent-1-en-3-one (E,Z isomer mixture) and 139 g (0.5 mol) of S-methylisothiourea sulphate were suspended in 2.5 liters of ethanol and 336 g (4 mol) of sodium bicarbonate were added in portions, while stirring. The mixture was heated under reflux for 4 hours, cooled to room temperature and poured onto water. The organic constituents were extracted with methylene chloride. The organic phase was dried over sodium sulphate, filtered and evaporated down. The resulting oil was caused to crystallize by stirring it with diisopropyl ether, and the crystals were recrystallized from ethanol. 42 g (12% of theory) of 1-(4-chlorophenyl)-4,4-dimethyl-1-methylthio-2-(1,2,4-triazol-1-yl)-pentan-3-one of melting point 145° C. were obtained. ##STR13## Process variant (c):

Provenance & Evidence