HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 6-bromo-N,N-dimethylquinoline-2-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 6-Bromoquinoline-2-carboxylic acid | HCID 12386208 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 6-bromo-N,N-dimethylquinoline-2-carboxamide | HCID 58119358 | 90.2% |
Reaction Steps
Suspended the 6-bromoquinoline-2-carboxylic acid (1.0 g, 3.93 mmol) in CH2Cl2 (20 mL), added DMF (0.91 mL, 11.78 mmol) and cooled in an ice bath. Added oxalyl chloride (0.688 mL, 7.86 mmol) dropwise over a few min. Warmed to rt and stirred for 1 hr then bubbled in dimethylamine gas for several min. The dark amber mixture was stirred at rt overnight. In am, the solution was diluted with water and extracted with CH2Cl2 (3×). Washed extracts with brine (1×), dried over MgSO4, decolorized with charcoal, filtered, evaporated and dried under high vac, rt to afford the title compound (990 mg). LC/MS: m/e 279, 281 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673941B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-7a918a273914490ab45f26b0f9350757 |
| Source note | uspto-grants-2014_03 |