HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2,6-Trimethyl-4H-1,3-dioxin-4-one → HCID 14801608, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2,6-Trimethyl-4H-1,3-dioxin-4-one | HCID 79368 | — |
| Reactant | Methyl (azepan-2-ylidene)acetate | HCID 67871225 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 14801608 | HCID 14801608 | 77% |
Reaction Steps
A mixture of 20.0 g of methyl α-(hexahydro-2-azepinylidene)acetate and 77 ml of xylene was gently refluxed, to which a mixture of 41.9 g of 2,2,6-trimethyl-4H-1,3-dioxin-4-one and 41 ml of xylene was dropwise added taking 45 minutes and refluxed for 2 hours, removing the by-product acetone through a Dean-Stark apparatus. The reaction mixture was cooled to room temperature. The resulting crystals were filtered, washed and dried to afford 21.4 g (Yield 77%) of methyl 2,6,7,8,9,10-hexahydro-4-methyl-2-oxo-pyrido[1,2-a]azepine-1-carboxylate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04936121 |
| Source dataset | uspto-grants-1990_06 |
| ORD ID | ord-8fef781350ce4a4b87c98ca361f94ac4 |
| Source note | uspto-grants-1990_06 |