Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | Carbamide Peroxide | HCID 31294 | — |
| Reactant | HCID 86720751 | HCID 86720751 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86720750 | HCID 86720750 | 75.5% |
Reaction Steps
To a chloroform (10 mL) solution of 2,5-dimethyl-5-nitropyridine (1.2 g), under ice cooling in a nitrogen atmosphere, carbamide peroxide (1.9 g) and trifluoroacetic anhydride (2.3 mL) were added dropwise, and the resultant was stirred for 30 minutes under ice cooling and then stirred at room temperature for 13 hours. Water was added to the reaction mixture, followed by extraction with chloroform. The obtained organic layer was washed with a 10% aqueous sodium thiosulfate solution and then dried over sodium sulfate, and the desiccant was filtered off. Then, the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (OH-type silica gel; chloroform/ethyl acetate-gradient elution=100/0→0/100) to obtain the title compound (1.0 g) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09045466B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-fc0d780bd6fb4834b8cd4c4dca110449 |
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| Source note | uspto-grants-2015_06 |
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