Water → HCID 12323798, compound

Participants

Reaction Steps

10.0 g (0.2 mol) of hydrazine hydrate, dissolved in 20 ml of dimethylformamide, were added dropwise to a solution of 26.7 g (0.1 mol) of 1-phenyl-1-ethoxycarbonyl-4-chloro-4-ethyl-2,3-diazabutadiene in 100 ml of dimethylformamide at a temperature of 5°C to 10°C, whilst stirring. After stirring for 3 hours, 250 ml of water were added to the reaction mixture. The whole was left to stand overnight. Thereafter, the solid which had precipitated was filtered off, well rinsed with water and dried. The yellowish-white crude product (17.4 g = 80% of theory) was purified by recrystallization from isopropanol/water. 14.5 g (67.1% of theory) of 3-ethyl-4-amino-6-phenyl-5-H-1,2,4-triazin-5-one of melting point 164°C were obtained.

Provenance & Evidence