5-butyl-2,2-dimethyl-1,3-dioxane-4,6-dione

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

実験手順: The 5-butyl-2,2-dimethyl-1,3-dioxane-4,6-dione thus obtained was allowed to reflux in ethanol for 2 hours, and then concentrated under reduced pressure. The resulting residue was purified using silica gel chromatography (developing solvent: n-hexane/ethyl acetate=8/2) to obtain the ethyl 3-oxohexanoate shown by the formula below. concentrated under reduced pressure The resulting residue was purified

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

実験手順: Meldrum's acid (2,2-dimethyl-1,3-dioxane-4,6-dione, 6.15 g, 42.7 mmol) and triethyl amine (8.63 g, 85.4 mmol) were dissolved in dichloromethane (60 mL). Butyric acid chloride (4.99 g, 46.9 mmol) was added to the solution thus obtained dropwise while cooling with ice, followed by stirring at room temperature for about 12 hours. The reaction mixture was concentrated under reduced pressure, and then the resulting residue was subjected to extraction using ethyl acetate. The thus-obtained organic layer was washed with dilute hydrochloric acid and an aqueous saturated sodium chloride solution, dried over magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was purified using silica gel chromatography (developing solvent: n-hexane/ethyl acetate=8/2) to obtain 5-butyl-2,2-dimethyl-1,3-dioxane-4,6-dione. thus obtained dropwise while cooling with ice The reaction mixture was concentrated under reduced pressure the resulting residue was subjected to extraction The thus-obtained organic layer was washed with dilute hydrochloric acid an aqueous saturated sodium chloride solution, dried over magnesium sulfate concentrated under reduced pressure The resulting residue was purified