HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 23510774, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 23510773 | HCID 23510773 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | HCID 23510774 | HCID 23510774 | 80.94% |
Reaction Steps
Ethyl 1-methyl-4-[2-(4-trifluoromethyl-phenylsulfanyl)-ethoxycarbonylamino]-1H-imidazole-2-carboxylate (0.69 g, 1.65 mmol) prepared in the capping step was dissolved in THF/H2O (27.40 ml/13.70 ml), 1N LiOH (4.57 ml) was added thereto, and the mixture was stirred at room temperature. After 15 hours have passed, the reaction solution was acidified to pH 2.0 by 1N HCl and then extracted with EA and water. The organic layer was washed with aqueous NaCl solution, dried over anhydrous MgSO4, and concentrated. The residue was recrystallized from EA and n-hexane to give 1-methyl-4-[2-(4-trifluoromethyl-phenylsulfanyl)-ethoxycarbonylamino]-1H-imidazole-2-carboxylic acid (0.52 g, 80.94%) of a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06759511B2 |
| Source dataset | uspto-grants-2004_07 |
| ORD ID | ord-207a690ac1ec41ccb6734b12dbb40251 |
| Source note | uspto-grants-2004_07 |