反应详情

温度

0 °C

A solution of 4-chloro-3-iodopyridin-2-amine (0.25 g, 0.982 mmol, Boa Pharma) in concd H2SO4 (1.95 mL) was cooled to about 0° C. before the portion wise addition of potassium nitrate (0.21 g, 2.2 mmol) over 10 min. The reaction was stirred for about 4 h at about 0° C. The reaction mixture was slowly pipetted over a solution of ammonium hydroxide and crushed ice (10 mL) in an ice bath. The pH of the reaction was maintained above 9 by the incremental addition of ammonium hydroxide. The resulting precipitate was filtered and dried to afford 4-chloro-3-iodo-5-nitropyridin-2-amine (0.085 g, 29%) as a green-tinted solid LC/MS (Table 1, Method n) Rt=0.64 min; MS m/z: 298 (M−H)−.

1. filtrationThe resulting precipitate was filtered
2. customdried