反应详情

A solution of 4-amino-6-(methyl-phenyl-amino)-[1,3,5]triazine-2-carbonitrile (Intermediate 2, 138 mg, 0.6 mmol) in EtOH (4 mL) was added to a solution of hydroxylamine hydrochloride (51 mg, 0.7 mmol) and sodium hydrogencarbonate (61 mg, 0.73 mmol) in water (2 mL). The mixture was heated at 70 C for 2 h, allowed to cool to room temperature and the solvent evaporated. The crude solid residue was slurried with water (4 mL) before filtering under reduced pressure to afford Intermediate 1 (95 mg, 60%). Method C HPLC-MS: MH+ requires m/z=260. Found: m/z=260, Rt=0.88 min (98%).

1. temperatureThe mixture was heated at 70 C for 2 h
2. customthe solvent evaporated
3. filtrationbefore filtering under reduced pressure