HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → HCID 66901659, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 66901760 | HCID 66901760 | — |
| Catalyst | Trifluoroacetic acid | HCID 6422 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66901659 | HCID 66901659 | — |
Reaction Steps
To a solution of 6-[(4-tert-butylphenyl)sulfonyl]-7-chloro-2-(trifluoromethyl)-6,11-dihydro-5H-pyrido[2,3-b][1,5]benzodiazepine (intermediate 25, 60 mg, 0.121 mmol) in DCM (1 mL) was added NBS (23.7 mg, 0.133 mmol) and a few drops of TFA. After stirring at rt for 3 h, the reaction mixture was concentrated to dryness, and the residue was dissolved in ether, washed with sodium thiosulfate, water and brine, dried over MgSO4, filtered and concentrated. The residue was purified by reverse phase HPLC to provide the title compound. LC/MS: m/e 574 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08153626B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-ffdaefdeca9346b5aa89260eeb89a16b |
| Source note | uspto-grants-2012_04 |