HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 1,3,4,5-Tetrahydro-4-(methoxyphenyl)-3-(2-propenyl)-7-(trifluoromethyl)-2H-1-benzazepin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Lithium iodide | HCID 66321 | — |
| Reactant | 1,3,4,5-Tetrahydro-3-(methoxycarbonyl)-4-(methoxyphenyl)-3-(2-propenyl)-7-(trifluoromethyl)-2H-1-benzazepin-2-one | HCID 20135113 | — |
| Catalyst | Water | HCID 962 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | 1,3,4,5-Tetrahydro-4-(methoxyphenyl)-3-(2-propenyl)-7-(trifluoromethyl)-2H-1-benzazepin-2-one | HCID 21290542 | 104.7% |
Reaction Steps
Lithium iodide (1.08 g; 8.04 mmole) was added to 1,3,4,5-tetrahydro-3-(methoxycarbonyl)-4-(methoxyphenyl)-3-(2-propenyl)-7-(trifluoromethyl)-2H-1-benzazepin-2-one (870 mg; 2.01 mmole) in pyridine (14 ml), three drops of water were added, and the mixture was refluxed with stirring for 6.5 hours. The solution was dissolved into ethyl acetate and washed with 1N hydrochloric acid (three times). The organic layer was dried (magnesium sulfate) and concentrated giving 0.79 g of solid. The crude material was used "as is" in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04752645 |
| Source dataset | uspto-grants-1988_06 |
| ORD ID | ord-3b4a2353da2640579fdcf9d06a5173b5 |
| Source note | uspto-grants-1988_06 |