HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Benzyl-4-piperidone → HCID 68832454, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Benzyl-4-piperidone | HCID 19220 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 4-Bromo-1,2-difluorobenzene | HCID 67675 | — |
| Reactant | Magnesium | HCID 5462224 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68832454 | HCID 68832454 | 48.8% |
Reaction Steps
To a suspension of 7.55 g of magnesium in 50 ml of THF is added dropwise a solution of 50 g of 1-bromo-3,4-difluorobenzene in 100 ml of THF so as to reach and then maintain reflux, and the mixture is left at reflux for 2 hours with stirring. After cooling to rt, a solution of 49 g of 1-benzyl-4-piperidinone in 100 ml of THF is added dropwise and the mixture is then stirred at RT overnight. The reaction mixture is poured onto saturated NH4Cl solution and extracted with ether, the organic phase is dried over Na2SO4 and the solvent is evaporated under vacuum. 38.3 g of the expected product are obtained after crystallization from cyclohexane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07521449B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-caa1e0ff25b94b6e91d5181de1b5b476 |
| Source note | uspto-grants-2009_04 |