Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | HCID 49764905 | HCID 49764905 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 49764778 | HCID 49764778 | 93.9% |
Reaction Steps
After dissolving 1.1 g of 5-(4-methylpentan-2-yl)-4-nitrotetrahydrothiophen-3-yl acetate in 7 ml of toluene, the solution was cooled to 4° C. A solution prepared by dissolving 0.8 g of sulfuryl chloride in 2 ml of toluene was added thereto. The temperature of the solution was allowed to rise room temperature, and the solution was stirred for 2 hours. Water was added to stop reaction, and the organic layer was washed with 1 mol/l aqueous sodium hydroxide and saturated saline. The organic layer was dried with magnesium sulfate and concentrated, and then purified by silica gel chromatography (hexane/ethyl acetate=10/1), thereby obtaining 0.8 g of 2-(4-methylpentan-2-yl)-3-nitrothiophene (yield: 85.0%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08367846B2 |
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| Source dataset | uspto-grants-2013_02 |
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| ORD ID | ord-c07f38563aa84a7c8d254f34f2ce0ef2 |
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| Source note | uspto-grants-2013_02 |
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