HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon tetrabromide → 4-(Bromomethyl)-1-(4-fluorophenyl)pyrrolidin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 1-(4-Fluorophenyl)-4-(hydroxymethyl)pyrrolidin-2-one | HCID 10465677 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | 4-(Bromomethyl)-1-(4-fluorophenyl)pyrrolidin-2-one | HCID 21935487 | — |
Reaction Steps
To a cooled solution of 1-(4-fluorophenyl)-4-(hydroxymethyl)pyrrolidin-2-one (0.05 g, 0.25 mmol) in pyridine (3 ml) was added triphenylphosphine (0.130 g, 0.5 mmol). The solution was stirred and carbon tetrabromide (0.08 g, 0.25 mmol) was added in 3 separate portions. The reaction mixture was then allowed to warm to room temperature and stirred for three hours. The reaction was quenched with methanol and the solvent removed. The residue was dissolved in EtOAc (75 ml) and sequentially washed with ammonium chloride (sat, 2×25 ml) and water (25 ml). The organic layer was concentrated and purified using preparative tlc (1:1 EtOac:Hexanes) to yield 4-(bromomethyl)-1-(4-fluorophenyl)pyrrolidin-2-one (HNMR).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07452889B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-93f60da592cc408aa40bfb6a22ddf852 |
| Source note | uspto-grants-2008_11 |