HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69725509, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Carbonate Ion | HCID 19660 | — |
| Reactant | 3,4-Dihydro-6-methyl-2H-pyran-2-one | HCID 138034 | — |
| Reactant | HCID 11789279 | HCID 11789279 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 69725509 | HCID 69725509 | 80.9% |
Reaction Steps
1.39 g of 5-acetonyl-3-methylisoxazole, 1.68 g of 3,4-dihydro-6-methyl-2H-pyran-2-one and 3.42 g of cecium carbonate were added to 20 ml of acetonitrile to heat at reflux for 3 hours. After returning to room temperatrure, the reaction solution was poured into 100 ml of ice water with hydrochloric acid added, and extracted with ethyl acetate. The organic layer was washed with water and then with saturated salt water, and dried over magnesium sulfate. The solvent was concentrated under reduced pressure. The obtained crude product was purified on silica gel column chromatography to give 2.03 g of the title compound as a colorless viscous liquid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06359143B1 |
| Source dataset | uspto-grants-2002_03 |
| ORD ID | ord-a597d167768949509dc3517ccd024bb7 |
| Source note | uspto-grants-2002_03 |