HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4,5-Bis(4-methoxyphenyl)-2-(4-trifluoromethylphenylthio)imidazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Isoamyl Nitrite | HCID 8053 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 4,5-Bis(4-methoxyphenyl)-2-(2-amino-4-trifluoromethylphenylthio)imidazole hydrochloride | HCID 20275408 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4,5-Bis(4-methoxyphenyl)-2-(4-trifluoromethylphenylthio)imidazole | HCID 12832305 | 85.7% |
Reaction Steps
2.61 g of 4,5-bis(4-methoxyphenyl)-2-(2-amino-4-trifluoromethylphenylthio)imidazole hydrochloride is suspended in a mixture of 70 ml of absolute ethanol, 30 ml of absolute dioxane, and 365 mg of hydrochloric acid and combined at 0° with 0.586 g of isoamyl nitrite. The mixture is agitated for 30 minutes, then heated for 2 hours to boiling, and the solution evaporated to dryness under vacuum. The residue is distributed between ethyl acetate and sodium bicarbonate solution. The organic solution is dried over sodium sulfate and concentrated to dryness under vacuum. The residue is crystallized from ether/methylene chloride, thus obtaining 2.01 g of 4,5-bis(4-methoxyphenyl)-2-(4-trifluoromethylphenylthio)imidazole, mp 184°-186°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04402960 |
| Source dataset | uspto-grants-1983_09 |
| ORD ID | ord-a61144376c734e84b322c8e2d56d2f37 |
| Source note | uspto-grants-1983_09 |