Potassium cyanate → HCID 135578191, compound

Participants

Reaction Steps

To a stirred mixture of 5.0 g (0.023 mole) of acetaldehyde 4-chloro-3-nitrophenylhydrazone in 50 ml of acetic acid was added dropwise a solution of 1.95 g (0.024 mole) of potassium cyanate in 5 ml of water. The resultant mixture was stirred at 15° C. for 1.5 hour. An additional 0.25 g (0.0031 mole) of potassium cyanate in 2 ml of water was added dropwise. This mixture was stirred for one hour. While maintaining a temperature of 15° C., 42.9 ml of an aqueous, 5% sodium hypochlorite solution was added dropwise. The resultant mixture was stirred at 15° C. for one hour. The solvents were removed by distillation under reduced pressure leaving a solid residue. This solid was stirred in 100 ml of toluene. The solvent was removed by evaporation under reduced pressure leaving a solid residue. The solid residue was dissolved in 150 ml of ethyl acetate. This solution was washed in succession with an aqueous, saturated sodium bicarbonate solution, water, and an aqueous, saturated sodium chloride solution. The washed organic phase was dried over anhydrous magnesium sulfate and was filtered. The filtrate was evaporated under reduced pressure to yield 5.77 g of 4,5-dihydro-3-methyl-1-(4-chloro-3-nitrophenyl)-1,2,4-triazol-5(1H)-one as a solid.

Provenance & Evidence