HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus tribromide → HCID 86680609, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 86680608 | HCID 86680608 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 86680609 | HCID 86680609 | 81.6% |
Reaction Steps
To a solution of 1-(5-(3-methoxyphenyl)pyridin-2-yl)propan-1-ol (0.45 g, 1.8 mmol) in chloroform (5 mL) was added PBr3 (1.5 g, 5.55 mmol) at 0-5° C., the reaction was maintained at the same temperature for 1 h, and then the reaction was slowly warmed to rt and maintained at this temperature for 1 h. The contents were diluted with water (75 mL) and chloroform (100 mL) and the layers were separated. The organic layer was washed with bicarbonate solution (2×30 mL), dried over sodium sulphate and distilled to get the crude product. The non-polar impurity was removed by pentane washings (2×7 mL) to provide 2-(1-bromopropyl)-5-(3-methoxyphenyl)pyridine (0.45 g, crude). LC-MS m/z calcd for [M+H]+ 306.04. found 306.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09199975B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-680010e9387a45218032444ef8ec38dc |
| Source note | uspto-grants-2015_12 |