Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 10593803 | HCID 10593803 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 15086293 | HCID 15086293 | — |
Reaction Steps
0.182 mol of ethyl acetoacetate is added at 0° C. to a suspension containing 0.182 mol of sodium hydride in 800 ml of tetrahydrofuran. The reaction medium is maintained for one hour at 20° C. and 0.182 mol of sodium iodide is then added. The mixture is cooled to 0° C. and 0.182 mol of 4-[bis(4-fluorophenyl)methylene]-1-(chloroethyl)piperidine is added. The mixture is brought to reflux for 12 hours and then concentrated under vacuum. The residue is taken up in water and the product is extracted with dichloromethane. The oil obtained is purified by chromatography on a column of 70-230 mesh silica, eluting with a mixture of dichloromethane and methanol (99:1 V/V).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05079249 |
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| Source dataset | uspto-grants-1992_01 |
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| ORD ID | ord-bc5bc2572c854b7d9335d66cabca1a73 |
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| Source note | uspto-grants-1992_01 |
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