HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → Methyl 3-cyclobutyl-3-oxopropanoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2,2-Dimethyl-1,3-dioxane-4,6-dione | HCID 16249 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 3-cyclobutyl-3-oxopropanoate | HCID 52911251 | — |
Reaction Steps
22 g of meldrum's acid (2,2-dimethyl-1,3-dioxane-4,6-dione) (152.7 mmol) and 36.9 ml of pyridine (457.2 mmol) were dissolved in 200 ml of dichloromethane. 18.1 g of cyclobutylcarbonic acid chloride were added at 0 to 10° C. The reaction mixture was stirred overnight at room temperature, washed with 1 N HCl and extracted with dichloromethane. The organic layer was washed with water, dried over magnesium sulfate, filtered, and then concentrated to dryness. The oily residue was dissolved in 300 ml of methanol and heated under reflux for 2 h. The reaction mixture was concentrated to dryness and the residue purified via silica gel chromatography with ethyl acetate as eluent. Yield: 21.2 g
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08101754B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-3523dd0c83744d1baeec6e5b154b4821 |
| Source note | uspto-grants-2012_01 |