HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon tetrabromide → 5-(2,2-Dibromovinyl)-2-methylpyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 6-Methyl-3-pyridinecarboxaldehyde | HCID 10192566 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-(2,2-Dibromovinyl)-2-methylpyridine | HCID 59455163 | 70% |
Reaction Steps
6-Methylnicotinaldehyde (1.0 g, 0.00826 mol) was dissolved in DCM (100 mL). Carbon tetrabromide (5.48 g, 0.0165 mol) and triphenylphosphine (8.66 g, 0.033 mol) was added to the solution followed by stirring at RT for 3 h. Insoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified through column chromatography (8% EtOAc:hexane in silica 100-200 mesh, diameter of column—5.0 cm, height of silica—approx. 5 inch) to provide the desired compound as a yellow colored oil (1.6 g, 70% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08907097B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-b3f237d1f92c4ed598769d7a0d61aff2 |
| Source note | uspto-grants-2014_12 |