HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 58494891, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 2,3,4,5-Tetrahydro-1H-benzo(d)azepine | HCID 1400243 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58494891 | HCID 58494891 | — |
Reaction Steps
To a solution of 1.75 g of 2,3,4,5-tetrahydro-1H-3-benzazepine in 20 ml of dichloromethane was added 2.884 ml of pyridine. The reaction mixture was ice-cooled, and 1.705 ml of ethyl chloroformate which had been dissolved in 5 ml of dichloromethane was added dropwise thereto, followed by stirring overnight. The reaction mixture was concentrated under reduced pressure and the residue was purified by silica gel chromatography (elution solvent: HEX-EtOAc) to obtain 2.15 g of ethyl 1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate as a pale yellow oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09108977B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-93406dd2c9d941eea68a38c7d3f3e78d |
| Source note | uspto-grants-2015_08 |