Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 4-Iodobenzenesulfonyl chloride | HCID 7399 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 11150443 | HCID 11150443 | 94% |
Reaction Steps
A solution of sodium carbonate (9.4 g, 74.375 mmol) in water (30 mL, 10 v/w) was dropwise added to a solution of 4-iodo-benzenesulfonyl chloride (3 g, 9.917 mmol) in 1,4-dioxane (15 mL, 5 v/w) at room temperature, followed by stirring at room temperature for 30 min. Then, 1N aqueous sodium hydroxide was dropwise added thereto so as to adjust the pH of the reaction mixture to 14, followed by stirring at room temperature for 12 hours. The reaction mixture was cooled to 0° C., and conc. H2SO4 solution was dropwise to adjust the pH of the reaction mixture to 1. The reaction mixture was extracted three times with ethyl acetate, and the organic layer thus obtained was washed with water. The washed layer was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to obtain the title compound (2.5 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08853213B2 |
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| Source dataset | uspto-grants-2014_10 |
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| ORD ID | ord-727395fbf8e046f1987a453c0a80888b |
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| Source note | uspto-grants-2014_10 |
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