Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfolane | HCID 31347 | — |
| Reactant | Potassium Fluoride | HCID 522689 | — |
| Reactant | HCID 69831429 | HCID 69831429 | — |
| Product | HCID 69831923 | HCID 69831923 | 30.1% |
Reaction Steps
A mixture of 3-(6-methoxy-m-tolyl)-6-chloro-5-nitro-1,2-benzisothiazole (7.30 g, 0.0218 mol), potassium fluoride (6.33 g, 0.109 mol) 18-crown-6 (2.31 g, 0.0872 mol) and sulfolane is stirred 19 hours at 154° C., cooled to room temperature, and poured into ice water. The resultant solid is filtered and chromatographed on silica gel with methylene chloride to afford a solid which is recrystallized from acetonitrile to afford a tan powder. The powder is recrystallized from ethyl acetate to give the title compound as a tan solid (2.09 g, 29.9%) which is identified by NMR spectral analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06355796B1 |
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| Source dataset | uspto-grants-2002_03 |
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| ORD ID | ord-fe912e9d1e164693af65f246fa6a8dac |
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| Source note | uspto-grants-2002_03 |
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