Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydroxylamine HCl | HCID 21645 | — |
| Reactant | HCID 135982142 | HCID 135982142 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178492115 | HCID 178492115 | 39.3% |
Reaction Steps
After adding 114 mg of hydroxylammonium chloride and 267 μl of triethylamine to a solution of 146 mg of 2-{3-[(4-cyanophenylamino)-(6-fluoro-9-methoxy-3,4-dihydro-2H-benzo[b][1,4]dioxepin-7-yl)methyl]-5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl}nicotinic acid in 10 ml of methanol, the mixture was heated for 28 hours at 60° C. After cooling the reaction mixture, it was purified by reverse-phase high performance liquid chromatography (acetonitrile-water, 0.1% acetic acid) to give the title compound (61 mg) as a light yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07816522B2 |
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| Source dataset | uspto-grants-2010_10 |
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| ORD ID | ord-bdfae69fb9464874a98e9dd7590ce298 |
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| Source note | uspto-grants-2010_10 |
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