Trifluoroacetic acid → 2,4-Dihydro-4-methyl-5-(trifluoromethyl)-3H-1,2,4-triazole-3-thione

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Reaction Steps

257 g (2.44 mol) of 4-methyl-thiosemicarbazide are added to 1.2 liters of trifluoroacetic acid, and the mixture is refluxed for 16 hours. It is then concentrated under a water pump vacuum, the residue is triturated with diethyl ether/petroleum ether (5:100 by volume), and the product, which is obtained as crystals, is isolated by filtration. 444.5 g (95.5% of theory) of 4-methyl-5-trifluoromethyl-2,4-dihydro-3H-1,2,4-triazole-3-thione of melting point 115° C. are obtained.

Provenance & Evidence