HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-Acetyl-4-(2',4'-difluorobenzoyl)piperidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,3-Difluorobenzene | HCID 9741 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 1-Acetylpiperidine-4-carbonyl chloride | HCID 100950 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-Acetyl-4-(2',4'-difluorobenzoyl)piperidine | HCID 2740707 | 41% |
Reaction Steps
67 g of 1,3-difluorobenzene and 133 g of ammonium chloride were added to 150 ml of dichloromethane, and then the mixture was cooled to room temperature. 98 g of 1-acetyl-4-piperidinecarbonyl chloride in 50 ml of dichloromethane was added thereto dropwise, and then the mixture was stirred at an elevated temperature for 3 hours. The reaction mixture was poured to a mixture of ice and hydrochloric acid, and the resulting mixture was extracted with 200 ml of dichloromethane. The organic phase was separated, dried over anhydrous magnesium sulfate, filtered, and the solvent was removed from the filtrate to obtain 55.9 g of the title compound (yield: 41%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07202360B2 |
| Source dataset | uspto-grants-2007_04 |
| ORD ID | ord-8f5e55c335594cdb9da2e72c9b389815 |
| Source note | uspto-grants-2007_04 |