Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 54498760 | HCID 54498760 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86756021 | HCID 86756021 | 100% |
Reaction Steps
A stirred solution of 6-fluoro-2-methyl-4-oxo-7-trifluoromethyl-3,4-dihydro-2H-quinoline-1-carboxylic acid isopropyl ester (940 mg, 2.8 mmol), hydroxylamine hydrochloride (215 mg, 3.1 mmol), and sodium acetate (254 mg, 3.1 mmol) in ethanol (20 mL) was heated at reflux for 3 h. Water (25 mL) was added, and the volatiles were removed in vacuo. Ethyl acetate (100 mL) was added, and the mixture was stirred vigorously for 10 min. The aqueous phase was separated and extracted with ethyl acetate (2×100 mL). The combined organic layers were washed with brine (100 mL), dried over sodium sulfate, filtered and concentrated in vacuo to give the title compound as a white foam (937 mg, ca. 100%): 1H NMR (CDCl3) δ 1.1 (d, 3H), 1.28 (d, 3H), 1.34 (d, 3H), 2.73 (dd, 1H), 3.09 (d, 1H), 5.0-5.1 (m, 2H), 7.68 (d, 1H), 7.88 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06395751B1 |
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| Source dataset | uspto-grants-2002_05 |
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| ORD ID | ord-4ad01914176049e98d15bf1509f67746 |
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| Source note | uspto-grants-2002_05 |
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