HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus tribromide → 4'-(Bromomethyl)-2'-fluorobiphenyl-2-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2'-Fluoro-4'-(hydroxymethyl)biphenyl-2-carbonitrile | HCID 67009990 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4'-(Bromomethyl)-2'-fluorobiphenyl-2-carbonitrile | HCID 67008432 | 100% |
Reaction Steps
To a solution (150 mL) of 2′-fluoro-4′-(hydroxymethyl)biphenyl-2-carbonitrile (14.1 g) in toluene was added phosphorus tribromide (18.7 g) at room temperature, and the mixture was stirred for 16 hr. Saturated aqueous sodium hydrogen carbonate was added to the reaction mixture, and the solvent was evaporated under reduced pressure, and the residue was extracted with ethyl acetate, and the obtained ethyl acetate layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound as a colorless solid (15.3 g, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08592431B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-aa8385a123824036a41433ecae4d5267 |
| Source note | uspto-grants-2013_11 |