Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | HCID 178432964 | HCID 178432964 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178432647 | HCID 178432647 | 84% |
Reaction Steps
5-Bromo-6-methylpicolin-imido-hydrazide (1 equiv) and formic acid (15 equiv) were combined and heated with stirring at 100° C. for 6 h. The reaction was cooled to room temperature and diluted with methanol. The resulting slurry was stirred for 30 min and then partially concentrated under reduced pressure to ˜20% of the total volume. The resulting mixture was again diluted with methanol and partially concentrated under reduced pressure to ˜20% of the total volume. The resulting solids were collected by filtration, washed three times with water and dried under reduced pressure to provide the desired product in 84% yield, as an off-white solid. MS (ESI) m/z 238.9 [M]+, 240.9 [M+2]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08569494B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-cc9e6d97fb434aa5b040808254e08e42 |
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| Source note | uspto-grants-2013_10 |
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