Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetone | HCID 180 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Sodium Sulfite | HCID 24437 | — |
| Reactant | 3,5-Dimethylisoxazole-4-sulfonyl chloride | HCID 2736319 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 23697072 | HCID 23697072 | 101.1% |
Reaction Steps
A solution of sodium sulfite (680 mg, 5.40 mmol) in water (5 mL) was added to an acetone (5 mL) solution of 3,5-dimethylisoxazole-4-sulfonyl chloride (530 mg, 2.70 mmol). The mixture was heated to 80° C., then a solution of sodium carbonate (430 mg, 4.05 mmol) in water (5 ml) was added dropwise. The mixture was refluxed for 16 hours then evaporated to dryness. The residue was refluxed with ethanol (20 mL), the inorganics were removed by filtration. Evaporation of the filtrate afforded 500 mg of crude sodium 3,5-dimethylisoxazole-4-sulfinate. It was used in the next steps without further purification. 1H NMR (400 MHz, DMSO-d6): δ 2.37 (s, 3H) and 2.22 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08293919B2 |
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| Source dataset | uspto-grants-2012_10 |
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| ORD ID | ord-16cc4349b324424487aa1cf4f126e3ad |
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| Source note | uspto-grants-2012_10 |
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