Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Potassium Iodide | HCID 4875 | — |
| Reactant | Potassium Iodate | HCID 23665710 | — |
| Reactant | HCID 178418479 | HCID 178418479 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | HCID 178524773 | HCID 178524773 | — |
Reaction Steps
6-Hydroxynicotinic acid (20 g) in water (200 ml) and H2SO4 (80 ml) was heated to 90° C. for 1 hour. Potassium iodate (0.42 equivalent) and potassium iodide (0.96 equivalent) were both added portionwise over 2 hours. After a further hour at 90° C. the mixture was cooled to 60° C. and added to 1 kg of ice. The brown solid was filtered off, dried and taken up in DMF (30 ml)/EtOH(1 litre). Sodium metabisulfite was added until the brown colour disappeared and the mixture was poured onto ice (2 kg), a further 1.5 litre water added and the white solid filtered to give title compound (16.5 g). NMR δ(DMSO) 12.95 (1H, broad), 12.35 (1H, broad), 8.36 (1H, d), 8.03 (1H, d)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06972297B2 |
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| Source dataset | uspto-grants-2005_12 |
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| ORD ID | ord-4d1cf850ac544cdda7fec36221f94862 |
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| Source note | uspto-grants-2005_12 |
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