Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | HCID 118113267 | HCID 118113267 | — |
| Product | HCID 118113302 | HCID 118113302 | — |
Reaction Steps
To a solution in ethanol (5.31 mL) of the compound (270 mg) obtained in step (1) above, cesium carbonate (346 mg) was added and the mixture was stirred at room temperature for an hour. The reaction mixture was concentrated under reduced pressure and 1 mol/L hydrochloric acid was added to the resulting residue. Extraction was conducted with ethyl acetate and the combined organic layers were dried over anhydrous sodium sulfate. After removing the desiccant by filtration, the filtrate was concentrated under reduced pressure. To a solution of the resulting concentrate (253 mg) in chloroform (4.88 mL), trifluoroacetic acid (2.44 mL) was added and the mixture was stirred at room temperature for 15 hours. After concentrating under reduced pressure, the residue was recrystallized with a liquid mixture of n-hexane and ethyl acetate and the precipitate was recovered by filtration to give the titled compound as a colorless solid (335 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09422240B2 |
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| Source dataset | uspto-grants-2016_08 |
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| ORD ID | ord-dff1497797ed40848df9a2685db64b3a |
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| Source note | uspto-grants-2016_08 |
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