HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 66939389, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | ethyl 1-{[4-(3-{[(acetyloxy)acetyl]amino}phenyl)-1,3-thiazol-2-yl]methyl}-1H-pyrazole-4-carboxylate | HCID 66939480 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 66939389 | HCID 66939389 | 48.7% |
Reaction Steps
To a solution (4 mL) of the compound (270 mg, 0.63 mmol) obtained in Example 45a in ethanol was added 2N aqueous sodium hydroxide solution (1.7 mL, 3.4 mmol), and the mixture was stirred at room temperature overnight. The reaction mixture was neutralized with 1N aqueous hydrochloric acid solution, saturated brine was added, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The resulting crude title compound was recrystallized (tetrahydrofuran-ethyl acetate-hexane) to give the title compound (110 mg, 33%) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461348B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-5398be2d458343989c1b01455782f7cc |
| Source note | uspto-grants-2013_06 |