Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 15105335 | HCID 15105335 | — |
| Reactant | HCID 15105352 | HCID 15105352 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 19746019 | HCID 19746019 | 31.2% |
Reaction Steps
2-(2-Chloroethyl)-5,6,7,8-tetrahydro-1,2,4-triazolo[4,3-a]-pyridin-3(2H)-one (2.08 g), 3.1 g of sodium iodide and 100 mλ of acetonitrile were refluxed for 30 minutes, and 3.1 g of 4-[bis(4-methoxyphenyl)methylene]piperidine and 2.8 g of potassium carbonate were added thereto, followed by refluxing for 18 hours. The insoluble material was removed by filtration, and the filtrate was concentrated to dryness under reduced pressure. The residue was dissolved in 100 mλ of chloroform, and the solution was applied to a column contained with 130 g of silica gel and eluted with a 15:1 (by volume) mixture of chloroform and ethanol. The eluate was concentrated to dryness, and the resulting residue was dissolved in ethanol, of concentrated hydrochloric acid was added thereto, followed by concentration to dryness. The residue was recrystallized from a mixture of ethanol and ethyl ether to obtain 0.85 g of the entitled compound as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05232924 |
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| Source dataset | uspto-grants-1993_08 |
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| ORD ID | ord-f66feef64f954baba09cc6c3bad1bd81 |
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| Source note | uspto-grants-1993_08 |
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