HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 18432004, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-Fluorobiphenyl | HCID 9461 | — |
| Reactant | 1-Acetylpiperidine-4-carbonyl chloride | HCID 100950 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 18432004 | HCID 18432004 | 80.8% |
Reaction Steps
12.5 g of acetyl-4-piperidinecarbonyl chloride were added portionwise to a mixture of 10 g of 4-fluoro-1,1′-biphenyl, 17.5 g of aluminum-(III)-chloride and 60 g of 1,2-di-chloroethane. Upon completion, stirring was continued for 1 hour at reflux temperature. The reaction mixture was poured into a mixture of crushed ice and hydrochloric acid. The product was extracted with DCM. The extract was dried, filtered and evaporated. The residue was crystallized from 2-propanol. The product was filtered off and dried, yielding 15 g (80.8%) of 1-acetyl-4-[(4′-fluoro-[1,1′-biphenyl]-4-yl]carbonyl]piperidine (interm. 3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06440440B1 |
| Source dataset | uspto-grants-2002_08 |
| ORD ID | ord-930383670b8a45adaccba25df3a959fa |
| Source note | uspto-grants-2002_08 |