Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | HCID 70873482 | HCID 70873482 | — |
| Reactant | HCID 86709368 | HCID 86709368 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 70874438 | HCID 70874438 | 41% |
Reaction Steps
A mixture of toluene-4-sulfonic acid (R)-4-(2-chloro-4-nitroimidazol-1-yl)-2-hydroxybutyl ester (1.16 g), 1-(4-hydroxyphenyl)-4-(4-trifluoromethylphenyl)piperidin-4-ol (1.0 g), tripotassium phosphate (2.52 g) in ethanol (10 ml) was stirred at 60° C. for 15 hours under an argon atmosphere. The reaction mixture was added to an ammonium chloride aqueous solution, and the mixture was stirred for a while. The precipitated crude crystal was collected by filtration and dried at 60° C. The crude product thus obtained was purified by silica gel column chromatography (methylene chloride:ethyl acetate=1:1) and recrystallized from acetone-water to afford the title compound as a beige powder (0.63 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09051333B2 |
|---|
| Source dataset | uspto-grants-2015_06 |
|---|
| ORD ID | ord-d83583073cec48f7ae40d7e35272299b |
|---|
| Source note | uspto-grants-2015_06 |
|---|