Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 178492115 | HCID 178492115 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 135982116 | HCID 135982116 | — |
Reaction Steps
To a solution of 61 mg of 2-(3-{(6-fluoro-9-methoxy-3,4-dihydro-2H-benzo[b][1,4]dioxepin-7-yl)-[4-(N-hydroxycarbamimidoyl)phenylamino]methyl}-5-oxo-4,5-dihydro-[1,2,4]triazol-1-yl)nicotinic acid in 6 ml of a methanol:water:acetic acid=1:1:1 mixed solvent there was added 60 mg of iron powder, and the mixture was stirred at 60° C. for 30 hours under a nitrogen atmosphere. Upon cooling, the reaction mixture was filtered through celite and purified by reverse-phase high performance liquid chromatography (acetonitrile-water, 0.1% trifluoroacetic acid) to give 2-{3-[(4-carbamimidoylphenylamino)-(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.
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-1dfbb59423e941789307c8ca63a4972d |
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| Source note | uspto-grants-2010_10 |
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