HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → HCID 15457065, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | HCID 15457188 | HCID 15457188 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | HCID 15457065 | HCID 15457065 | 81.4% |
Reaction Steps
2.63 g (8.23 mmol) of 3-(4-chloro-2-fluoro-5-methylphenyl)-1-methyl-6-trifluoromethyl-2(1H)-pyridone and 1.46 g (8.23 mmol) of NBS were dissolved in 100 ml of carbon tetrachloride. Then, 0.27 g (1.67 mmol) of 2,2′-azobisisobutyronitrile was slowly added thereto with stirring under heating and refluxing. Then, the mixture was further reacted for 5 hours. After cooling, the insoluble substances were filtered off, and the organic layer was washed with water and dried over magnesium sulfate. The solvent was distilled off under reduced pressure. Then, the obtained residue was purified by silica gel column chromatography to obtain 2.67 g (yield: 81%) of the desired product. Melting point: 117-118° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06472348B1 |
| Source dataset | uspto-grants-2002_10 |
| ORD ID | ord-f791307be7e24c318c05ee31b13d5165 |
| Source note | uspto-grants-2002_10 |