Acetic Anhydride → HCID 71293873, compound

Participants

Reaction Steps

In pyridine (2.0 mL) was dissolved 1-(5-bromopyridin-3-yl)-2,2,2-trifluoroethanol (390 mg, 1.52 mmol) obtained in Step 2. Acetic anhydride (2.0 mL) was added and the mixture was stirred at room temperature for 18 hours. The solvent was evaporated under reduced pressure and a saturated aqueous sodium bicarbonate solution and water were added. Extraction with ethyl acetate, washing with saturated brine 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 (hexane/ethyl acetate=1/1) and further purified by preparative thin-layer chromatography (hexane/ethyl acetate=4/1) to give 1-(5-bromopyridin-3-yl)-2,2,2-trifluoroethyl acetate (429 mg, 95% yield).

Provenance & Evidence