HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → 5-(Bromomethyl)-2-chloro-3-fluoropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 2-Chloro-3-fluoro-5-methylpyridine | HCID 13541365 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | 5-(Bromomethyl)-2-chloro-3-fluoropyridine | HCID 59297078 | 48% |
Reaction Steps
A suspension of 2-chloro-3-fluoro-5-methylpyridine (5.1 g, 35 mmol), N-bromosuccinimide (6.1 g, 35 mmol) and benzolyperoxide (0.16 g, 0.66 mmol) in carbon tetrachloride (100 mL) was refluxed overnight. Upon cooling down, the solid was filtered off and the filtrate was concentrated and loaded onto a silica gel column eluted with 5% EtOAc in hexane to give 3.77 g of the desired 2-chloro-3-fluoro-5-bromomethylpyridine as colorless oil in 48% yield. GC-MS calcd. for C6H4BrClFN: 224.46. Found: 224.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08178565B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-3bfdfc11e9e240edb48b595e62955d33 |
| Source note | uspto-grants-2012_05 |