HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 131719-68-1
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | HCID 10396924 | HCID 10396924 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 131719-68-1 | HCID 15752625 | 61% |
Reaction Steps
To a stirred solution of (E)-3-cyclohexyl-2-propen-1-ol (A. G. M. Barrett et al, Tetrahedron, 1996, 52, 15325), (1.47 g, 10.5 mmol) in diethyl ether (20 ml) and pyridine (1 ml) was added phosphorus tribromide (1.40 ml, 15 mmol) dropwise at room temperature under an atmosphere of nitrogen. After 16 h, the reaction mixture was carefully poured onto ice water (100 ml) and extracted with diethyl ether (100 ml). The extract was washed with saturated aqueous sodium hydrogen carbonate solution (100 ml), dried (MgSO4) and concentrated in vacuo to give the crude product. This was purified by silica (20 g) column chromatography eluting with hexane:ethyl acetate (4:1) to give the title compound as a colourless oil (1.3 g, 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06610711B2 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-1aedfde6431c48ad8cefd83a1cec963f |
| Source note | uspto-grants-2003_08 |