Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | O-(2,4-dinitrophenyl)hydroxylamine | HCID 87140 | — |
| Reactant | HCID 15457186 | HCID 15457186 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 15457050 | HCID 15457050 | 68% |
Reaction Steps
10 ml of DMF was added to 0.10 g of 60% sodium hydride, and 0.72 g of 3-(2,4-dichlorophenyl)-6-trifluoromethyl-2(1H)-pyridone was added thereto under cooling with ice, followed by stirring further at room temperature for 30 minutes. Then, 0.47 g of 2,4-dinitrophenoxyamine was added thereto at room temperature. Then, the mixture was stirred at 50° C. for 1 hour to complete the reaction. After completion of the reaction, the reaction solution was washed with water and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and then, the solvent was distilled off to obtain a crude product. This crude product was purified by silica gel column chromatography to obtain 0.50 g (yield: 68%) of the desired product. Melting point: 98-100° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06472348B1 |
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| Source dataset | uspto-grants-2002_10 |
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| ORD ID | ord-a2bcb9a62b4d41e394801c10f37f3f9b |
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| Source note | uspto-grants-2002_10 |
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