Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22031472 | HCID 22031472 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178504677 | HCID 178504677 | 48.8% |
Reaction Steps
A mixture of 58 mg 4-(5-methylsulfonyl 2-thienyl)-6-(3-trifluoromethyl-1-trityl-1H-4-pyrazolyl)qui noline obtained in Example 158, 1 mL trifluoroacetic acid and 3 mL dichloromethane was stirred overnight at room temperature. The reaction solution was cooled with iced water and basified with 5 N aqueous sodium hydroxide, then ethyl acetate and water were added thereto, and the organic layer was separated. The aqueous layer was then extracted with ethyl acetate, and the combined organic layer was washed with water and an aqueous brine and dried over anhydrous sodium sulfate. The drying agent was filtered off, and the filtrate was evaporated. The residue was triturated with diethyl ether, and the crystals were separated by filtration to give 18 mg of the title compound as pale yellow crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07074801B1 |
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| Source dataset | uspto-grants-2006_07 |
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| ORD ID | ord-8e9681b48a2a4fe0a4a041faf7fe326a |
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| Source note | uspto-grants-2006_07 |
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