Sulfuric Acid → HCID 178441961, compound

Participants

Reaction Steps

First 5.12 kg (50 mols) of acetic anhydride and then 2.78 kg (25 mols) of pivaloyl cyanide were introduced, in each case at room temperature, into 9.81 kg (100 mols) of concentrated sulphuric acid which had been initially introduced into the reaction vessel. After subsequently stirring this reaction mixture for 2 hours, it was stirred into a solution of 2.66 kg (25 mols) of thiocarbohydrazide in 30 liters of 1 N HCl at 20°-30° C. When the addition had ended, the mixture was subsequently stirred for a further 2 hours at 50°-55° C.; after cooling, the reaction product which had precipitated was filtered off, washed with 20 liters of water and dried. 4.80 kg (96% of theory) of 4-amino-6-tert.-butyl-3-mercapto-1,2,4-triazin-5(4H)-one (V) were obtained as colorless crystals of melting point 212°-214° C.; content, according to determination by gas chromatography, >99%.

Provenance & Evidence