Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | HCID 57871042 | HCID 57871042 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 57870886 | HCID 57870886 | 30% |
Reaction Steps
150 mg (0.503 mmol) of ethyl 6-[N-(1H-pyrrol-1-yl)sulfamoyl]-1-cyclohexene-1-carboxylate obtained in Example 31 was dissolved in 3 ml of tetrahydrofuran, and 70 mg (0.528 mmol) of N-chlorosuccinimide was added thereto with stirring under ice-cooling, followed by stirring overnight at room temperature. Water was added to the reaction solution and the mixture was extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate, followed by concentration under reduced pressure. The residue was subjected to silica gel thin layer chromatography (solvent; hexane:ethyl acetate=2:1) and the resulting solid was further washed with isopropyl ether to give 50 mg of the title compound as a white powder (yield: 30%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07935835B2 |
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| Source dataset | uspto-grants-2011_05 |
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| ORD ID | ord-c07b18e1d18947edb1bcae910a251d88 |
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| Source note | uspto-grants-2011_05 |
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