HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 119086060, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 1,2,3,4-Tetrahydro-benzo(b)azepin-5-one | HCID 294788 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 119086060 | HCID 119086060 | 67.7% |
Reaction Steps
A mixture of 1,2,3,4-tetrahydro-1-benzazepin-5-one (500 mg, 2.530 mmol), O-methyl hydroxylamine hydrochloride (211 mg, 2.530 mmol), sodium acetate (208 mg, 2.530 mmol) and sodium carbonate (536 mg, 5.060 mmol) in ethanol was refluxed for 3 hours. The resulting mixture was concentrated in vacuo to remove ethanol and to the residue was added water (15 mL). The residue in water was extracted with dichloromethane (15 mL×3). The organic layers were combined, dried over sodium sulfate, and concentrated in vacuo to afford 326 mg of the desired product (yield was 67%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08871756B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-4362013957b946a79274110c85bb1904 |
| Source note | uspto-grants-2014_10 |