Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Oxalic Acid | HCID 971 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 178466643 | HCID 178466643 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 178465685 | HCID 178465685 | — |
Reaction Steps
A solution of 0.125 g (1.81 mmol) of hydroxylamine hydrochloride and 0.5 g (0.006 mol) of sodium acetate in 10 ml of water is stirred for 10 minutes, and a solution of 0.125 g (0.512 mmol) of 4-[3-(3-ethanoylphenoxy)propyl]-1H-imidazole in 3 ml of ethanol is then added slowly. The mixture is stirred at room temperature for 1 hour and then heated at 80° C. for 2 hours. After cooling, the solvent is removed under reduced pressure and the white residue obtained is extracted with chloroform. The chloroform is dried (MgSO4) and then evaporated. The oil obtained is dissolved in 4 ml of 2-propanol and treated with 1.3 equivalents of oxalic acid in 3 ml of 2-propanol. The addition of diethyl ether yields the product, which is separated by filtration, washed with ether and recrystallized in a 2-propanol/diethyl ether mixture, m.p. 149-151° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06248765B1 |
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| Source dataset | uspto-grants-2001_06 |
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| ORD ID | ord-792d3f31801446b492d7c8c1382c4a29 |
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| Source note | uspto-grants-2001_06 |
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