HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 2,6-Difluoro-beta-oxo-benzenepropanoic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 2,2-Dimethyl-1,3-dioxane-4,6-dione | HCID 16249 | — |
| Reactant | 2,6-Difluorobenzoyl chloride | HCID 87438 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2,6-Difluoro-beta-oxo-benzenepropanoic acid methyl ester | HCID 20148994 | — |
Reaction Steps
To 3.6 g (25 mmole, 1 eq) of Meldrum's acid and 6.1 g of 4-dimethylamino-pyridine in 60 ml of methylenechloride was added with stirring, 4.4 g (25 mmole) of 2,6-difluorobenzoylchloride. The temperature was maintained at 0° throughout the addition period and for three additional hours of stirring under argon atmosphere. Most of the methylene chloride was then removed by distillation at 25° or less using a water aspirator to maintain reduced pressure. There was then added 60 ml of anhydrous methanol containing 25 mmole of conc. sulfuric acid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04729782 |
| Source dataset | uspto-grants-1988_03 |
| ORD ID | ord-2e41e3ecd2274b329cc2477bc76cc104 |
| Source note | uspto-grants-1988_03 |