Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Hydroxylamine HCl | HCID 21645 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 57749243 | HCID 57749243 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 57749251 | HCID 57749251 | 167.7% |
Reaction Steps
A mixture of ethyl {[(5-{3-[(tert-butoxycarbonyl)amino]-4-methylphenoxy}pyridin-2-yl)amino]carbonothioyl}carbamate (11.5 g, 15.4 mmol), hydroxylammonium chloride (15.4 g, 0.223 mol), N,N-diisopropylethylamine (23.0 mL, 0.132 mol), ethanol (200 mL) and methanol (200 mL) was stirred at 80° C. for 12 hr. The reaction solution was concentrated under reduced pressure and ethyl acetate was added to the residue. The mixture was washed with water and saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure, and the residue was recrystallized from ethyl acetate-hexane to give the title compound (9.18 g, 100%) as a white 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-6cb6db0feb914e08acc3db5d93d14b85 |
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| Source note | uspto-grants-2012_11 |
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