HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 1-Bromomethyl-2-fluoro-4-phenoxy-benzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | (2-Fluoro-4-phenoxyphenyl)-methanol | HCID 57656488 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-Bromomethyl-2-fluoro-4-phenoxy-benzene | HCID 57656013 | 72% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
Dissolve under nitrogen atmosphere (2-fluoro-4-phenoxyphenyl)-methanol (1.41 g, 6.5 mmol) in anhydrous THF (60 mL). Cool to 0° C. in an ice bath. Add phosphorous tribromide (2.11 g, 7.8 mmol). Stir at cold for 1 h, then remove the ice bath and stir at ambient temperature for 16 h. Quench the reaction with saturated aqueous NaHCO3. Extract aqueous phase three times with EtOAc. Combine organic fractions, wash with brine, dry over Na2SO4 and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (9:1). Evaporate the solvent to obtain the title compound (1.31 g, 72%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022062B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-4845a7d1cea045ff8234255979561388 |
| Source note | uspto-grants-2011_09 |