HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 18319513, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Phosphorus pentachloride | HCID 24819 | — |
| Reactant | HCID 18319582 | HCID 18319582 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18319513 | HCID 18319513 | 91.9% |
Reaction Steps
Under nitrogen atmosphere, phosphorus pentachloride (1.6 g) was added to a mixture of methyl 2,3-dihydro-9-hydroxymethyl-1-benzoxepin-4-carboxylate (1.2 g) and pyridine (0.62 ml) in dichloromethane (24 ml) under ice-cooling and the mixture was stirred at the same temperature for 2 hours. To the reaction mixture was added a mixture of ethyl acetate and water. The separated organic layer was washed with saturated aqueous sodium bicarbonate and water. The organic layer was dried over magnesium sulfate and evaporated in vacuo to give methyl 2,3-dihydro-9-chloromethyl-1-benzoxepin-4-carboxylate (1.19 g) as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06346527B1 |
| Source dataset | uspto-grants-2002_02 |
| ORD ID | ord-4efd4229a6c84a6296a04116b64cef6e |
| Source note | uspto-grants-2002_02 |