Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | HCID 70873338 | HCID 70873338 | — |
| Reactant | HCID 86709368 | HCID 86709368 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 70874844 | HCID 70874844 | 75.4% |
Reaction Steps
Toluene-4-sulfonic acid (R)-4-(2-chloro-4-nitroimidazol-1-yl)-2-hydroxybutyl ester (988 mg) and 4-(4-{2-[N-methyl-N-(4-trifluoromethoxyphenyl)amino]ethyl}piperidin-1-yl)phenol (1.0 g) were suspended in ethanol (30 ml). Tripotassium phosphate (1.08 g) and sodium iodide (418 mg) were added to the suspension, and the mixture was stirred at 80° C. under a nitrogen atmosphere for 4.5 hours. After being cooled to room temperature, ethyl acetate (20 ml) was added to the reaction mixture, insoluble matter was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1→methylene chloride:methanol=97:3) to afford the title compound as a reddish brown oil (1.17 g).
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-d7055b55971440fcb167daeab21aa4e3 |
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| Source note | uspto-grants-2015_06 |
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