HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Fluoro-3-methylbutan-2-one → 1,1-Dibromo-3-fluoro-3-methyl-2-butanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Fluoro-3-methylbutan-2-one | HCID 12531590 | — |
| Reactant | Pyridiniumtribromide | HCID 21124087 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1,1-Dibromo-3-fluoro-3-methyl-2-butanone | HCID 22240099 | 72.1% |
Reaction Steps
To a stirred solution of 3-methyl-3-fluoro-2-butanone (0.1031 g, 0.990 mmol) in anhydrous dichloromethane (5 ml) under nitrogen was added solid pyridinium tribromide (0.7035 g, 1.98 mmol) and the mixture was stirred at room temperature for 18 h. The mixture was then diluted with dichloromethane (5 ml), washed with dilute aqueous sodium hydrogensulfite (10 ml), then saturated aqueous NaCl (10 ml), dried (Na2SO4) and evaporated under low vacuum with no heat. The residue was purified by flash chromatography [silica gel, 5% Et2O/petroleum ether (40-60° C.)] to afford 0.1869 g (72%) of the title compound as a colourless oil: 1H NMR (360 MHz, CDCl3) δ 1.65 (6H, d, J 21.5 Hz), 6.51 (1H, d, J 1.5 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06617326B2 |
| Source dataset | uspto-grants-2003_09 |
| ORD ID | ord-85ebb76396bc4b54a474ba6729981dae |
| Source note | uspto-grants-2003_09 |