HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → 2-Bromo-5-bromomethylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 2-Bromo-5-methylpyridine | HCID 564216 | — |
| Reactant | 2-Bromo-5-(dibromomethyl)pyridine | HCID 56605143 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | 2-Bromo-5-bromomethylpyridine | HCID 6424660 | 43% |
Reaction Steps
To a stirred slurry of 10.320 g (60.0 mmol) of 5-methyl-2-bromopyridine and 5.339 g (30.0 mmol, 0.5 eq) of recrystallized N-bromosuccinimide in 150 mL of carbon tetrachloride was added 200 mg of AIBN. The reaction mixture was purged twice with argon and evacuated and set to reflux under argon. After 90 min, the reaction mixture was cooled to room temperature, filtered and the filtrate concentrated to give a yellow oil. Proton NMR indicated that the mixture contains 53% (mol) unreacted 5-methyl-2-bromopyridine, 43% of the title product and 4% of 2-bromo-5-(dibromomethyl)pyridine. The mixture was used immediately without further purification for the following procedure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07534763B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-6837e4d7239d435188e20e7fc663e976 |
| Source note | uspto-grants-2009_05 |