Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | HCID 86709368 | HCID 86709368 | — |
| Reactant | HCID 86709370 | HCID 86709370 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86709369 | HCID 86709369 | 35.5% |
Reaction Steps
Toluene-4-sulfonic acid (R)-4-(2-chloro-4-nitroimidazol-1-yl)-2-hydroxybutyl ester (848 mg) and 4-[4-(tert-butyl-dimethylsilanyloxy)[1,4′]bipiperidinyl-1′-yl]phenol (850 mg) were suspended in ethanol (30 ml). Tripotassium phosphate (1.02 g) and sodium iodide (359 mg) were added to the suspension, and the mixture was stirred at 75° C. for 3 hours under a nitrogen atmosphere. After being cooled to room temperature, the reaction mixture was concentrated under reduced pressure, and water was added to the resulting residue, followed by extraction with ethyl acetate. The organic layer was dried over sodium sulfate and concentrated under reduced pressure. Insoluble matter that was precipitated by adding isopropyl ether to the residue was collected by filtration to afford the title compound as a pale brown powder (470 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09051333B2 |
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| Source dataset | uspto-grants-2015_06 |
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| ORD ID | ord-2d07d5f868b94b6d960ddae6cbf9ac86 |
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| Source note | uspto-grants-2015_06 |
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