Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thiophenol | HCID 7969 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 68159452 | HCID 68159452 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66938707 | HCID 66938707 | 84% |
Reaction Steps
The compound (260 mg, 0.365 mmol) obtained in step D was dissolved in acetonitrile (3 ml). Then, benzenethiol (0.057 ml, 0.547 mmol) and cesium carbonate (594 mg, 1.82 mmol) were added, and the mixture was stirred at room temperature for 10 hr. The reaction mixture was diluted with dichloromethane, and the organic layer was washed with diluted aqueous sodium hydroxide solution, and dried over anhydrous magnesium sulfate. The insoluble material was filtered off, and the solution was concentrated under reduced pressure. The obtained oil was purified by silica gel column chromatography (NH silica gel use, methanol-dichloromethane) to give the title compound (161 mg, yield 84%) as a pale-yellow amorphous solid. This was directly used for the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08513235B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-d015302b86814d2e83d466f845d8c0d2 |
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| Source note | uspto-grants-2013_08 |
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