Acetic Acid → HCID 178448762, compound

Participants

Reaction Steps

2.31 kg (15.88 moles) of chloropivaloyl cyanide were added to 9 liters of a solution of hydrogen bromide in glacial acetic acid (33% strength) at room temperature, while stirring. The mixture was subsequently stirred at room temperature for 4 hours. 288 ml (15.88 moles) of water were then added at 7° to 10° C. (exothermic reaction, about 37° C.) and the mixture was subsequently stirred at room temperature for 3 hours. Thereafter, the reaction solution was introduced into a mixture of 2.03 kg of thiocarbohydrazide and 15.9 liters of 1 N hydrochloric acid at 7° to 10° C. (highly exothermic reaction). This reaction mixture was subsequently stirred at 7° to 10° C. for 2 hours and at room temperature for 14 hours. Thereafter, the crystals which had precipitated were filtered off, washed with water and dried. 2,995 g (80.4% of theory) of crude 4-amino-6 -chloro-tert.-butyl-3-mercapto-1,2,4-triazin-5-one of melting point 202°-208° C. were obtained.

Provenance & Evidence