HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus tribromide → HCID 90460608, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 117607196 | HCID 117607196 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 90460608 | HCID 90460608 | 108.5% |
Reaction Steps
To a solution of (2-chloro-4-methoxy-5-nitrophenyl)methanol (5.0 g, 23 mmol) in dichloromethane (50 mL) at 0° C., tribromophosphine (3.08 g, 11.5 mmol) was added in portions and the resulting mixture was stirred at RT for 2 h. The mixture was poured into ice-water and extracted with dichloromethane. The organic layer was washed with brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (petroleum ether/ethyl acetate=10:1) to afford the desired product (3.5 g, 54.2% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09227978B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-30511eff0ddb4324872315159000d2e3 |
| Source note | uspto-grants-2016_01 |