Potassium Carbonate → HCID 71294095, compound

Participants

Reaction Conditions

Reaction Steps

In n-butanol (2 mL) was dissolved 1-(2-aminopyridin-4-yl)-2,2,2-trifluoroethyl acetate (53.2 mg, 0.227 mmol) obtained in Step 2. Bromoacetone (0.042 mL, 0.45 mmol) was added and the mixture was stirred at 130° C. for 24 hours. A saturated aqueous sodium bicarbonate solution and water were added to the reaction mixture. Extraction with ethyl acetate and drying over anhydrous sodium sulfate were performed. After filtration, the solvent in the filtrate was evaporated under reduced pressure and the residue was dissolved in methanol (2.0 mL). Potassium carbonate (31.4 mg, 0.227 mmol) was added and the mixture was stirred at room temperature for 18 hours. A saturated aqueous ammonium chloride solution was added to the reaction mixture. Extraction with ethyl acetate and drying over anhydrous sodium sulfate were performed. After filtration, the solvent in the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform/methanol=5/1) to give Compound A30 (20.7 mg, 40% yield).

Provenance & Evidence