Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 19365486 | HCID 19365486 | — |
| Product | HCID 19365540 | HCID 19365540 | 95% |
Reaction Steps
To 3.3 ml of concentrated sulfuric acid was added 0.50 g of 3-(4chloro-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine (present compound 1-11) at 5° C. Furthermore, 0.17 ml of 61% nitric acid was added, and the mixture was stirred at room temperature for 1 hour. After completion of the reaction, the reaction mixture was added to ice water, followed by extraction with ethyl acetate. The organic layer was washed with water and then saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography, which afforded 0.55 g (yield, 95%) of 3-(4-chloro-2-fluoro-5-nitrophenyl)-1-methyl-6-trifluoromethyl-2-oxo-1,2-dihydropyrazine (present compound 1-17; m.p., 98.3° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06015774 |
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| Source dataset | uspto-grants-2000_01 |
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| ORD ID | ord-d4169d2fb3a046b3b56832b9faee9148 |
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| Source note | uspto-grants-2000_01 |
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