HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus tribromide → HCID 57656575, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 57655910 | HCID 57655910 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 57656575 | HCID 57656575 | 83.3% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
Add phosphorous tribromide (1.45 g, 5.34 mmol) slowly to a solution of 1-(4-hydroxymethyl-phenoxy)-3,3-dimethylbutan-2-one (1.08 g, 4.85 mmol) in anhydrous THF under nitrogen at 0° C. Stir at 0° C. for 1 h and then raise to ambient temperature. Stir overnight. Dilute with EtOAc, wash with saturated aqueous NaHCO3, brine, dry over Na2SO4, filter and concentrate. Purify the residue by chromatography on silica gel eluting with EtOAc:hexane (1:6) to provide the title compound (1.152 g, 83%). MS (ES+) m/z: 205 (M-Br)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022062B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-cc8b3b504e074e809a7dfdbff5b62830 |
| Source note | uspto-grants-2011_09 |