HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 3,4-Dihydro-4,4-dimethyl-2H-pyran-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Ethyl 4-formyl-3,3-dimethylbutanoate | HCID 13050815 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 3,4-Dihydro-4,4-dimethyl-2H-pyran-2-one | HCID 3018685 | 40.1% |
Reaction Steps
A solution of 11.16 g (0.065 mole) of ethyl 3,3-dimethyl-5-oxopentanoate and 11.2 g (0.073 mole) of phosphoryl chloride in 90 ml of toluene was heated under reflux for 14 hours. The mixture was diluted with ether, washed with an aqueous solution of sodium bicarbonate, dried over anhydrous magnesium sulfate, filtered, and the filtrate concentrated to give, after distillation, 3.29 g (40% yield) of 3,4-dihydro-4,4-dimethyl-2H-pyran-2-one, bp 105°-110° C./2670 Pa (20 mm Hg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04344884 |
| Source dataset | uspto-grants-1982_08 |
| ORD ID | ord-77fb5c9d2f004ba8a6cb5829930cf35a |
| Source note | uspto-grants-1982_08 |