Hydrochloric Acid → 2-Amino-5-chloronicotinamide

Temperature

60 °C

(Step 1) To a solution of 2-aminonicotinamide (0.5 g) in concentrated hydrochloric acid (3 ml) was added dropwise 30% aqueous hydrogen peroxide (0.3 ml). After stirring at 60° C. for 1 hr, the reaction mixture was diluted with water and basified with 1N aqueous sodium hydroxide solution. The mixture was extracted with a mixed solution of ethyl acetate and THF, washed with saturated brine and dried over magnesium sulfate. The reaction solvent was concentrated under reduced pressure, and the residue was purified by silica gel chromatography (ethyl acetate) to give 2-amino-5-chloronicotinamide as crystals (0.25 g).

1. extractionThe mixture was extracted with a mixed solution of ethyl acetate and THF
2. washwashed with saturated brine
3. dry with materialdried over magnesium sulfate
4. concentrationThe reaction solvent was concentrated under reduced pressure
5. customthe residue was purified by silica gel chromatography (ethyl acetate)

ORD record

ord-6cca1587981b47e198ea63f4a72a8121

Source dataset

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08470859B2