Ethyl Acetate → HCID 68662288, compound

Participants

Reaction Steps

A solution of 2-amino-5-chloronicotinamide (150 mg) and 4-(bromomethyl)-3-fluorobenzonitrile (282 mg) in DMF (3 ml) was stirred at 100° C. for 24 hr. After cooling to room temperature, ethyl acetate was added, and the precipitated crystals were filtered. The obtained crystals were dissolved in methanol (3 ml) and partitioned between ethyl acetate and aqueous sodium hydrogen carbonate solution. The organic layer was dried over magnesium sulfate and filtered. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/methanol=1/0-9/1). 4N Hydrochloric acid-ethyl acetate solution was added to the obtained yellow oil, and the precipitated crystals were filtered and recrystallized to give the title compound (47 mg).

Provenance & Evidence