Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 178473690 | HCID 178473690 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178434758 | HCID 178434758 | — |
Reaction Steps
A mixture of 3-(2,4-pentanedion-3-yl)thio-1H-1,2,4-triazole (2 g), hydroxylamine hydrochloride (0.7 g), triethylamine (1.4 ml) and ethanol (10 ml) was heated and stirred for 5 hours on an oil bath at 100° C. The reaction solution was concentrated under reduced pressure, and then extracted with ethyl acetate-water. The organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to a silica-gel column chromatography with 10 to 30% (20% 2-propanol/ethyl acetate)/hexane, followed by recrystallization in ethyl acetate-hexane to yield the title compound (440 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07238720B2 |
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| Source dataset | uspto-grants-2007_07 |
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| ORD ID | ord-cc14cea576b8429bbe0f79f74156484d |
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| Source note | uspto-grants-2007_07 |
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