反应详情

温度

90 °C

A mixture containing 4-amino-3-nitrophenol (1 eq) and potassium bis(trimethylsilyl)amide (2 eq) was stirred in dimethylformamide for 2 hours at room temperature. To this mixture was added 4-Chloro-pyridine-2-carboxylic acid dimethylamide (1 eq) and potassium carbonate (1.2 eq) and then it was stirred at 90° C. for 3 days. The reaction mixture was then concentrated before partitioning between ethyl acetate and water. The organic layer was separated, washed with brine, dried, filtered and concentrated in vacuum to give brown solid. Purification by flash chromatography with ethyl acetate and hexane (1:1) gave the desired product as a yellow syrup. HPLC, 1.69 min; MS: MH+=303.1.

1. concentrationThe reaction mixture was then concentrated
2. custombefore partitioning between ethyl acetate and water
3. customThe organic layer was separated
4. washwashed with brine
5. customdried
6. filtrationfiltered
7. concentrationconcentrated in vacuum
8. customto give brown solid
9. customPurification by flash chromatography with ethyl acetate and hexane (1:1)