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

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.

1. customthus obtained dropwise
2. temperaturewhile cooling with ice
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. extractionthe resulting residue was subjected to extraction
5. washThe thus-obtained organic layer was washed with dilute hydrochloric acid
6. dry with materialan aqueous saturated sodium chloride solution, dried over magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe resulting residue was purified

ORD-Eintrag

ord-1f349d7513544363acf154a38eb848ed

Quelldatensatz

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08436210B2