Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen iodide | HCID 24841 | — |
| Reactant | HCID 57750963 | HCID 57750963 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 20152693 | HCID 20152693 | 65% |
Reaction Steps
A 57% aqueous solution of hydriodic acid (15 mL) was added to neat 3-nitro-thiophene-2-sulfonamide (1.02 g, 4.90 mmol) at room temperature. The reaction mixture was heated at 90° C. for 1 hour, cooled to room temperature and diluted with ethyl acetate (50 mL). The mixture was washed with a solution of sodium thiosulfate and the pH was adjusted to pH˜8 with sodium bicarbonate. The mixture was extracted with 10% methanol in ethyl acetate and the organic phase was dried over magnesium sulfate and concentrated in vacuo. Purification by column chromatography, using a gradient of 30-70% ethyl acetate in hexanes as the eluent, gave 65% yield of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09145380B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-944183c50aec48a7b5122936c9ab87e5 |
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| Source note | uspto-grants-2015_09 |
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