HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon tetrabromide → HCID 86628049, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 13208939 | HCID 13208939 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86628049 | HCID 86628049 | 84% |
Reaction Steps
To a solution of 2-[2-(4-cyanophenyl)ethoxy]ethanol (4.3 g, 0.0225 mol; see step (iv) above) in DCM (50 mL), triphenylphosphine (11.8 g, 0.045 mol) was added. The resulting mixture was stirred for 15 min and cooled to between 0 and 5° C. A solution of CBr4 (14.9 g, 0.045 mol) in DCM (25 mL) was added dropwise and the resulting mixture was stirred at room temperature overnight. The reaction mixture was concentrated and the crude product was purified by column chromatography (silica gel: 60-120 mesh, petroleum ether: ethyl acetate (70:30) eluent) to provide the title compound (yield: 4.8 g, 84%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928225B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-45832775836544f39c6cab0c321807d6 |
| Source note | uspto-grants-2011_04 |