Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 6-Nitroindazole | HCID 24239 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178526460 | HCID 178526460 | 85.1% |
Reaction Steps
Iodine (2.14 g, manufactured by Kanto Chemical Co., Inc.) and potassium hydroxide (475 mg, manufactured by Wako Pure Chemical Industries, Ltd.) were added to a solution of 6-nitro-1H-indazole (690 mg, manufactured by Wako Pure Chemical Industries, Ltd.) in N,N-dimethylformamide (20 mL, manufactured by Kanto Chemical Co., Inc.), and the mixture was stirred for one hour at room temperature. A saturated aqueous solution of sodium thiosulfate (20 mL) was added to the reaction solution, and the mixture was extracted with chloroform (3×20 mL), washed with brine (40 mL), and dried (MgSO4). The solvent was then evaporated. The resulting residue was purified by silica gel column chromatography (chloroform:methanol=9:1), to give 1.04 g of the title compound. LC-MS: HPLC retention time 0.54 minutes, m/z 290 (M+H), condition C-3.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07994202B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-8315ed848fcd45e8808ede473e834eef |
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| Source note | uspto-grants-2011_08 |
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