Ammonium → HCID 11806705, compound

Participants

Reaction Conditions

Reaction Steps

18.5 g (0.1 mol.) of cyanuric chloride was dissolved in 150 mL of acetonitrile. The solution was cooled to 0° C. and the cooled solution was dropwise added, while stirring, with a solution of 7.3 g (0.1 mol.) of butylamine in 20 mL of water over one hour in such a manner that the reaction temperature did not raise over 5° C. While further continuing the stirring, a solution of 10.0 g (0.1 mol.) of potassium hydrogencarbonate in 100 mL of water was dropwise added to the mixture at the same temperature and stirred for three hours. After the completion of the conversion of the resulting product into 2-butylamino-4,6-dichloro-1,3,5-tirazine was recognized by a high-performance liquid chromatography, 24.3 g (0.4 mol.) of an aqueous 28-% ammonium solution were added. The temperature was raised to 50° C. and the reaction was carried out for five hours. After the cooling, an obtained product was separated through filtration and washed fully with a large amount of water. An obtained crude product was suspended in 100 mL of water and added with 29.2 g (0.4 mol.) of butylamine and reacted for six hours under heating and refluxing. After the completion of the cooling, the resulting product was added with 200 mL of toluene and vigorously stirred and then, the aqueous layer was separated. Further, after the toluene layer was thrice washed with each 150 mL of water, toluene was distilled off from the organic layer under heating and reduced pressure to obtain 22.1 g of 2-amino-4,6-bis-(n-butylamino)-1,3,5-triazine (yield: 93%).

Provenance & Evidence