HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalic Acid → HCID 14032489, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalic Acid | HCID 971 | — |
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1,1'-(4-Chlorobutylidene)bis(4-fluorobenzene) | HCID 76820 | — |
| Reactant | (2-Fluoro-phenyl)-piperidin-4-yl-methanone | HCID 13180312 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 14032489 | HCID 14032489 | 34.6% |
Reaction Steps
A mixture of 10.0 g of 4-(2-fluorobenzoyl)piperidine, 16.9 g of potassium carbonate, 20.8 g of 4-chloro-1,1-bis(4-fluorophenyl)butane, 250 ml of dimethylformamide and a few crystals of potassium iodide was heated at 90° for 8 hrs with stirring. The reaction mixture was poured into water and extracted with ethyl acetate. The ethyl acetate extract was washed with water, dried over anhydrous magnesium sulfate and the solvent removed in vacuo to yield an oil. The oil was dissolved in ether, and oxalic acid was added. Recrystallization of the resultant solid from ethanol gave 10.6 g (34.6%) of 1-[4,4-bis(4-fluorophenyl)-1-butyl]-4-(2-fluorobenzoyl)piperidine oxalate, mp 179°-181° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04775761 |
| Source dataset | uspto-grants-1988_10 |
| ORD ID | ord-613fa95e3c4d4d97a0fa266497a6d1e4 |
| Source note | uspto-grants-1988_10 |