HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzoyl Peroxide → 2-Bromo-5-bromomethylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzoyl Peroxide | HCID 7187 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 2-Bromo-5-methylpyridine | HCID 564216 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | 2-Bromo-5-bromomethylpyridine | HCID 6424660 | — |
Reaction Steps
2-Bromo-5-methylpyridine (5.00 g, 29.1 mmoles) and N-bromosuccinimide (5.22 g, 29.3 mmoles) were dissolved in carbon tetrachloride (40 mL) under nitrogen. Benzoyl peroxide (0.35 g, 1.4 mmoles) was added and the mixture heated at reflux for four hours. The mixture was cooled to room temperature, filtered, and washed with NaHCO3/H2O. The mixture was adsorbed onto silica gel and then chromatographed. eluting with a gradient of hexane to 10% ethyl acetate/hexane. Pure fractions were combined and concentrated to provide the desired mono-brominated product as a pale yellow solid, 3.60 g (49%). LC/MS (M+H)+ m/z=249.8, 251.8, 253.8.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08697870B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-04125bc6e7ef4e8ca62f420316a53590 |
| Source note | uspto-grants-2014_04 |