Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | HCID 58201209 | HCID 58201209 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1209459-79-9 | HCID 58201198 | — |
Reaction Steps
5-Bromo-4-methoxy-2,3-dimethylpyridine 1-oxide (4.91 g) was dissolved in dichloromethane (60 ml), and trifluoroacetic anhydride (20 ml) was then added to the solution at room temperature. The resulting mixture was stirred overnight. Thereafter, the reaction solution was concentrated, and the concentrated solution was then dissolved in methanol (50 ml). The resulting mixture was stirred at 50° C. for 1 hour. The reaction solution was concentrated. The residue was dissolved in dichloromethane, and was then washed with a saturated sodium bicarbonate solution. The organic layer was dried over anhydrous sodium sulfate, and the filtrate was then concentrated. The residue was purified by silica gel column chromatography (hexane-ethyl acetate), so as to obtain the title compound (3.43 g) as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08445504B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-2e54e65aaf46461e8384b203d2aeae6d |
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| Source note | uspto-grants-2013_05 |
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