Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Hydroxylamine HCl | HCID 21645 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 57749328 | HCID 57749328 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 57749095 | HCID 57749095 | 70.1% |
Reaction Steps
A mixture of ethyl ({[5-(3-{[(1,3-dimethyl-1H-pyrazol-5-yl) carbonyl]amino}-4-fluorophenoxy)pyridin-2-yl]amino}carbonothioyl)carbamate (1.15 g, 2.43 mmol), hydroxylammonium chloride (1.18 g, 17.0 mmol), N,N-diisopropylethylamine (2.12 mL, 12.2 mmol), ethanol (10 mL) and methanol (10 mL) was stirred at 80° C. for 8 hr. The reaction mixture was diluted with water and extracted with ethyl acetate (×3). The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure, and the residue was collected by filtration and washed with ethyl acetate-hexane to give the title compound (650 mg, 70%) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08304557B2 |
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| Source dataset | uspto-grants-2012_11 |
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| ORD ID | ord-dfb65ee2f2e34f1fbbdd1ebd31f3a32f |
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| Source note | uspto-grants-2012_11 |
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