HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus tribromide → 1-[4-(2-Bromoethyl)piperidin-1-yl]-2,2-diphenylethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus tribromide | HCID 24614 | — |
| Reactant | 1-[4-(2-Hydroxyethyl)piperidin-1-yl]-2,2-diphenylethanone | HCID 58230382 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-[4-(2-Bromoethyl)piperidin-1-yl]-2,2-diphenylethanone | HCID 67416021 | 26.3% |
Reaction Steps
1-[4-(2-Hydroxyethyl)piperidin-1-yl]-2,2-diphenylethanone (2.39 g; 8.11 mmol) was dissolved in dichloromethane (20 ml). At room temperature, phosphorous tribromide (1.6 ml; 8.92 mmol) was slowly added dropwise. The reaction mixture was heated under reflux for 4 h. Cooling was followed by washing with saturated NaHCO3 solution, 2N HCl and saturated NaCl solution, and the organic phase was separated off and dried over Na2SO4. The solvent was removed under reduced pressure. Purification of the residue through a cartridge (silica gel) resulted in 1-[4-(2-bromoethyl)-piperidin-1-yl]-2,2-diphenylethanone (0.75 g; 2.13 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08710232B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-4274a8b147194b55bf55472c0d4dc76f |
| Source note | uspto-grants-2014_04 |