p-Toluenesulfonic acid → HCID 21399304, compound

Participants

Reaction Steps

Monomethylamine was passed for 4 hours into a boiling solution of 42.8 g of 4-amino-6-sec.-butyl-3-methylthio-1,2,4-triazin-5 (4H)-one of which 12 ml of glacial acetic acid and 1 g of p-toluenesulfonic acid had been added, and the mixture was then boiled for a further 4 hours under reflux. The solvent was largely evaporated off in vacuo and the oily residue was taken up in methylene chloride and repeatedly shaken with 10% strength sodium carbonate solution. The organic phase was separated off and concentrated by evaporation. 38.6 g (98% of theory) of 4-amino-6-sec.-butyl-3-methylamino-1,2,4-triazin-5 (4H)-one which gradually solidified, remained. The product was purified further by recrystallization from carbon tetrachloride. Melting point = 117° C.

Provenance & Evidence