反应详情

EDCI (2.30 g, 0.012 mol) and 1-hydroxy benztriazole (1.36 g, 0.009 mol) were added o a stirred solution of pyridine-2-carboxylic acid (1.0 g, 0.008 mol) in N,N-dimethyl formamide (16 mL) at 0° C. The reaction mixture was allowed to stir for 15 min then triethyl amine was added followed by addition of N,O-dimethyl hydroxyl amine hydrochloride at 0° C. The resulting mixture was stirred at RT overnight. The reaction mixture was partitioned between water (30 mL) and ethyl acetate (2×30 mL). The organic layer was dried over sodium sulphate and concentrated. The crude product was purified by column chromatography using 100-200 mesh silica gel and 0-20% EtOAc: Hexane as eluant to obtain product.

1. stirringThe resulting mixture was stirred at RT overnight
2. customThe reaction mixture was partitioned between water (30 mL) and ethyl acetate (2×30 mL)
3. dry with materialThe organic layer was dried over sodium sulphate
4. concentrationconcentrated
5. customThe crude product was purified by column chromatography
6. customHexane as eluant to obtain product