HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid monohydrate → HCID 15908406, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 22316766 | HCID 22316766 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 15908406 | HCID 15908406 | 63.9% |
Reaction Steps
A mixture of 4-hydroxy-1-[4-(methylsulfonyl)phenyl]-2-[4-(2-thienyl)phenyl]-4-(trifluoromethyl)-4,5-dihydro-1H-imidazole (0.345 g, 0.74 mmol) and p-toluenesulfonic acid monohydrate (0.035 g) in toluene (40 mL) was heated to reflux for 7 hours. The reaction mixture was cooled and the solvent removed under reduced pressure. The crude residue was redissolved in CH2Cl2 (50 mL) and the whole washed with water, aqueous NaHCO3 (30 mL), and brine. After dried over Na2SO4, and concentration in vacuo. The crude mixture was purified by flash chromatography eluting with hexane/ethyl acetate (2/1). The resulting solid was recrystallized from ethyl acetate-hexane to give the title compound (0.212 g, 63.9% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06949536B2 |
| Source dataset | uspto-grants-2005_09 |
| ORD ID | ord-11c4fb6dac574a1fad22dbe283571814 |
| Source note | uspto-grants-2005_09 |