2-(phenylhydrazinylidene)acetaldehyde

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a mixture of 2-(phenylhydrazono)ethanal (3.10 g) (Journal of Chemical Society, Perkin Trans. 1, 1981, 503-513.), potassium carbonate (4.40 g) and dioxane (20.0 mL) was added 1-chloropropan-2-one (2.10 g) at room temperature, and the mixture was heated under reflux for 5 hr. The reaction mixture was concentrated under reduced pressure and extracted with dichloromethane. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (dichloromethane/methanol) to give the title compound (1.35 g). the mixture was heated under reflux for 5 hr The reaction mixture was concentrated under reduced pressure extracted with dichloromethane The extract was washed with saturated brine dried over anhydrous sodium sulfate the solvent was evaporated under reduced pressure The residue was purified by silica gel column chromatography (dichloromethane/methanol)