反应详情

4-Cyanobenzaldehyde (3.0 g) was dissolved in a 1:1 mixed solution of ethanol/1,4-dioxane (80 mL), and bromoform (7.0 g) was added thereto under ice cooling. Subsequently, an ethanol solution (40 mL) of potassium hydroxide (7.6 g) was carefully added thereto, and the mixture was stirred for 6 hours at room temperature. After distilling off the solvent under reduced pressure, the residue thus obtained was diluted with water. The mixture was acidified with a 2 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 (2.6 g) was obtained as a crude product.

1. additionwas added
2. distillationAfter distilling off the solvent under reduced pressure
3. customthe residue thus obtained
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. distillationAfter distilling off the solvent under reduced pressure
8. customthe residue was purified by silica gel column chromatography (50% to 100% ethyl acetate/hexane)