Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Fumarate | HCID 5460307 | — |
| Reactant | 4-(3-Chloropropoxy)-3-methoxyacetophenone | HCID 7314264 | — |
| Reactant | HCID 15020370 | HCID 15020370 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 19983119 | HCID 19983119 | — |
Reaction Steps
A mixture of α,α-bis(4-fluorophenyl)-4-piperidineacetamide (6.94 g, 0.021 mole), 1-[4-(3-chloropropoxy)-3-methoxyphenyl]ethanone (5.09 g, 0.021 mole), and potassium carbonate (5.53 g, 0.04 mole) was heated overnight at reflux in 350 ml of 1-butanol containing potassium iodide (0.2 g). The mixture was concentrated to dryness. The residue obtained was partitioned between chloroform and water. The chloroform layer was dried (sodium sulfate) and filtered. The solvent was removed to give a yellowish-brown residue. This material was converted to the fumarate, and the salt was recrystallized from methanol-diethyl ether. A white solid was obtained and dried in vacuo overnight at 80° C. This method provided 8.47 g (66.8%) of white, crystalline product, mp 258°-260° C. (dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05070087 |
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| Source dataset | uspto-grants-1991_12 |
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| ORD ID | ord-1f9017279b634d0281123dffb9558a88 |
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| Source note | uspto-grants-1991_12 |
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