Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium Sulfite | HCID 24437 | — |
| Reactant | HCID 59331430 | HCID 59331430 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 59331526 | HCID 59331526 | 88.2% |
Reaction Steps
To a solution of 2-(4,5-diiodo-1H-imidazol-2-yl)pyridine (18.6 g) in a mixed solvent of N,N-dimethylformamide (200 mL) and water (100 ml) was added sodium sulfite (35.4 g), and the mixture was stirred at 120° C. for 24 hr. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed successively with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:99-20:80, volume ratio) to give the title compound (11.2 g, yield 88%) as colorless crystals. melting point 175-179° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08318746B2 |
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| Source dataset | uspto-grants-2012_11 |
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| ORD ID | ord-fc69744d7e0c41b8b006aaef2c7bd677 |
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| Source note | uspto-grants-2012_11 |
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