Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Naphthol | HCID 7005 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-(2-chloroethyl)-1H-imidazole hydrochloride | HCID 178478570 | — |
| Catalyst | Tetrabutylammonium Iodide | HCID 67553 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178419980 | HCID 178419980 | — |
Reaction Steps
240 mg (60% in oil, 6 mmol) of sodium hydride are added to a solution of 1.73 g (12 mmol) of 1-naphthol in 10 ml of dimethylformamide. The mixture is stirred at room temperature for 1 hour under nitrogen. 200 mg (1.2 mmol) of 4-(2-chloroethyl)-1H-imidazole hydrochloride and tetrabutylammonium iodide (catalytic amount) are added. The mixture is heated at 100° C. for 3 days and the solvent is then evaporated under reduced pressure. The remaining oily residue is taken up in dichloromethane and an aqueous sodium carbonate solution and treated with active charcoal. The dichloromethane solution is separated and evaporated and the remaining residue is chromatographed on a column of silica gel (10/1 dichloromethane/methanol) to give the title compound in the base form. The oxalate is prepared from isopropanol and is crystallized from ethanol, M.p.: 187°-189° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05559113 |
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| Source dataset | uspto-grants-1996_09 |
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| ORD ID | ord-38a9540c29f14a5aab25df2fe58c3c06 |
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| Source note | uspto-grants-1996_09 |
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