HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitric Acid → HCID 15457055, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | HCID 15457048 | HCID 15457048 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | HCID 15457055 | HCID 15457055 | 96% |
Reaction Steps
1.0 g (3.3 mmol) of 3-(4-chloro-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2(1H)-pyridone was dissolved in 10 ml of concentrated sulfuric acid, and 0.25 g (4.0 mmol) of fuming nitric acid was dropwise added thereto under cooling with ice, followed by stirring for 1 hour. This reaction solution was poured into ice water and extracted with ethyl acetate. After washing with water and a saturated sodium hydrogencarbonate aqueous solution, the organic layer was dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure, and then, the obtained residue was purified by silica gel column chromatography to obtain 1.1 g (yield: 96%) of the desired product. Melting point: 139-140° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06472348B1 |
| Source dataset | uspto-grants-2002_10 |
| ORD ID | ord-cc6562dd98a7486ea0a05fb401b26bf2 |
| Source note | uspto-grants-2002_10 |