HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → 4-Bromomethyl-2-fluoropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 2-Fluoro-4-methylpyridine | HCID 2737403 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 4-Bromomethyl-2-fluoropyridine | HCID 13985168 | 21.1% |
Reaction Steps
A solution of 2-fluoro-4-methylpyridine (0.5 g) in chloroform (50 ml) was treated with N-bromosuccinimide (1.35 g) and azobisisobutyronitrile (0.25 g). The mixture was heated at reflux for 30 hours, cooled to room temperature and washed with water (30 ml). The chloroform solution was evaporated and the resulting brown oil purified by flash chromatography on silica eluting initially with a mixture of ethyl acetate and pentane (1:9, v/v) then with a mixture of ethyl acetate and pentane (15:85, v/v). Fractions homogenous in the required product were combined and evaporated affording the title compound (0.18 g) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06048893 |
| Source dataset | uspto-grants-2000_04 |
| ORD ID | ord-0844d1423b5b4c2fa6bf7510ef71e3c1 |
| Source note | uspto-grants-2000_04 |