6-Chloro-5-iodo-3-nitropyridin-2-amine synthesis

Yield:790692-90-9 88%

Reaction Conditions:

with iodine;silver sulfate in ethanol at 20;

Steps:

5.a

To a suspension of 6-chloro-3-nitropyridin-2-amine (6.3 g, 36.3 mmol)in ethanol (110 ml_), 9.2 g (36.3 mmol) of iodine and 1 1.32 g (36.3 mmol) of silver sulphate were added. The crude mixture was stirred at room temperature overnight and the precipitate formed was filtered off. The solid isolated was purified by flash chromatography (1 :1 hexane/ethyl acetate) to give the title compound (9.74 g, 88% of yield). δ ¹H-NMR (CDCI₃): 1.56 (s, 2H), 8.76 (s, 1H).ESI/MS m/e: 300 ([IvH-H]⁺, C₅H₃CIIN₃O₂)

References:

WO2007/39297,2007,A1 Location in patent:Page/Page column 28