HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 59799037, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 59799046 | HCID 59799046 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Product | HCID 59799037 | HCID 59799037 | — |
Reaction Steps
Under a nitrogen atmosphere, mix 9-bromo-6-hydroxy-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (6 g, 17.8 mmol), anhydrous pyridine (0.06 mL, 0.72 mmol), 4-(dimethylamino)pyridine (222 mg, 1.8 mmol) and acetic anhydride (30 mL). Heat the mixture at reflux for 8 h and stir at RT for another 8 h Concentrate, dilute the residue in EtOAc, wash with 1 N HCl, and then with saturated aqueous sodium bicarbonate solution. Dry (sodium sulfate) and concentrate to give the title compound that was used in the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07981882B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-5db9ab45e79c4f3fb7431ecc69a27d13 |
| Source note | uspto-grants-2011_07 |