4214-73-7

1187322-51-5

Synthesis of 6-amino-5-iodonicotinonitrile: 6-amino-3-pyridinecarbonitrile (10.0 g, 0.081 mol), silver trifluoroacetate (25.5 g, 0.115 mol) and 1,2-dichloroethane (160 mL) were added to a flask and heated and refluxed for 5 hours. Iodine (29.5 g, 0.116 mol) was then added and heating and refluxing was continued for 18 hours. Upon completion of the reaction, the mixture was cooled, filtered, and partitioned between water and 1,2-dichloroethane. The organic and aqueous phases were filtered through diatomaceous earth, respectively. The aqueous phase was extracted repeatedly with 1,2-dichloroethane until depleted, the organic phases were combined, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was dissolved in ethyl acetate and washed with sodium thiosulfate solution. The solvent was removed under reduced pressure to give 6.6 g of pale yellow crystalline product, which could be used in the next reaction without further purification.HPLC retention time: 2.57 min; LCMS (m/z): 246 [M + H]+.