HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → Ethyl 7-bromo-2,3-dihydro-1-benzazepine-4-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Ethyl 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylate | HCID 18472216 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | Ethyl 7-bromo-2,3-dihydro-1-benzazepine-4-carboxylate | HCID 18472278 | 59% |
Reaction Steps
In 1N hydrochloric acid (25 ml) and ethanol (20 ml) was dissolved ethyl 7-bromo-1-formyl-2,3-dihydro-1-benzazepine-4-carboxylate (1165 mg), and the mixture was refluxed for 2 hours. The mixture was neutralized with saturated sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate (300 ml). The organic layer was washed with water (100 ml) and dried with anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified with silica gel column chromatography (150 g, hexane/ethyl acetate=9:1) to give ethyl 7-bromo-2,3-dihydro-1-benzazepine-4-carboxylate (628 mg, 59%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06166006 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-3ea26364206c40319e163fbc8411e62d |
| Source note | uspto-grants-2000_12 |