Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | HCID 19078333 | HCID 19078333 | — |
| Reactant | HCID 86751068 | HCID 86751068 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86751067 | HCID 86751067 | 80.9% |
Reaction Steps
A mixture of cyclopropyl-[4-(2-phenyl-1-imidazolyl)phenyl]methanone (2.6 g), aminoethylhydroxylamine dihydrochloride (1.95 g), and 3 equivalents of pyridine, in absolute ethanol (30 ml) was heated under reflux, under nitrogen, with stirring, overnight. The reaction mixture was evaporated, the residue was taken up in ethyl acetate and washed with a 10% sodium hydroxide solution. The organic extracts were evaporated and the residue purified by high performance liquid chromatography (silica gel, 185:14:1 dichloromethane/methanol/ammonium hydroxide). The appropriate fractions were collected and concentrated. The residue was taken up in ethanol and treated with ethereal hydrogen chloride. The mixture was evaporated. The residue was recrystallized from ethanol/ether to give 3.06 g (80.9%) of product, mp >220° C. (dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05648367 |
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| Source dataset | uspto-grants-1997_07 |
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| ORD ID | ord-4bb5f6894b944b42aac054e80a046bee |
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| Source note | uspto-grants-1997_07 |
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