Acetic Acid → HCID 178480783, compound

Participants

Reaction Conditions

Reaction Steps

A 250 mL round bottom flask was charged with 5-bromo-2-(4-methylpiperazin-1-yl)pyridine-3,4-diamine (1.2 g, 4.2 mmol) and CH3COOH (10 mL). To the above was added dropwise a solution of NaNO2 (0.30 g, 4.3 mmol) in water (1 mL) at 10° C. The resulting mixture was stirred at 10° C. for 1 h. Work-up: the reaction mixture was basified to pH 8 by saturated aqueous Na2CO3 and extracted with ethyl acetate (30 mL×3). The combined organic layers were dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel with 10% MeOH in CH2Cl2, to afford 1.1 g (88%) of the product as a white solid. MS m/z: 297 (M+H+).

Provenance & Evidence