HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → HCID 117770794, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 117770287 | HCID 117770287 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 117770794 | HCID 117770794 | 61.9% |
Reaction Steps
To a solution of 4-chloro-1-(2-chlorophenyl)-6-methyl-2-oxo-1,2-dihydropyridine-3-carbonitrile obtained in Step E (1.55 g) in carbon tetrachloride (69.4 mL) were added N-bromosuccinimide (1.19 g) and 2,2′-azobis(isobutyronitrile) (0.0910 g) at room temperature. The reaction mixture was refluxed for 3 hr, and cooled to room temperature. The reaction mixture was diluted with dichloromethane, and the mixture was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (1.23 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09085578B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-4815c41edbe141858921601c4fc5a448 |
| Source note | uspto-grants-2015_07 |