Methanol → HCID 21905685, compound

Participants

Reaction Steps

4-Trifluoromethoxybenzaldehyde (25.0 g) was dissolved in a 1:1 mixed solution of methanol/1,4-dioxane (500 mL), and bromoform (30.3 g) was added thereto under ice cooling. Subsequently, a methanol solution (150 mL) of potassium hydroxide (3.3 g) was added dropwise thereto, and the mixture was stirred for 22 hours at room temperature. After distilling off the solvent under reduced pressure, the residue was diluted with water. The mixture was acidified with 3 mol/L hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with saturated brine and then dried over anhydrous sodium sulfate. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (50% to 100% ethyl acetate/hexane), and the title compound (29.4 g) was obtained as a crude product.

Provenance & Evidence