Synthesis
General procedure for the synthesis of 3-amino-6-bromo-1,2,4-triazine from 1,2,4-triazin-3-amine: 3-amino-1,2,4-triazine (I) (0.96 g, 10 mmol) was dissolved in 100 mL of N,N-dimethylformamide (DMF) with thorough stirring. A 100 mL DMF solution of N-bromosuccinimide (NBS) (17.8 g, 100 mmol) was added slowly and dropwise under the cooling of an ice bath. The reaction temperature was maintained between 0-30 °C with continuous stirring for 12 hours. After completion of the reaction, sodium hydroxide (12 g, 300 mmol) was added to the reaction mixture for neutralization. The precipitate was collected by filtration and dried to afford the target product 3-amino-6-bromo-1,2,4-triazine (1.43 g, 81.7% yield).
References
[1] Patent: CN108129409, 2018, A. Location in patent: Paragraph 0043; 0044; 0045
[2] Journal of the American Chemical Society, 2015, vol. 137, # 26, p. 8388 - 8391
[3] Patent: US2016/251361, 2016, A1. Location in patent: Paragraph 1004-1006
[4] Russian Chemical Bulletin, 2014, vol. 63, # 6, p. 1359 - 1363
[5] Izv. Akad. Nauk, Ser. Khim., 2014, # 6, p. 1359 - 1363,5
