Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus pentachloride | HCID 24819 | — |
| Reactant | N-[2-amino-2,2-bis(4-fluorophenyl)-1-methylethyl]-2-pyrazinecarboxamide | HCID 69053565 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 178432625 | HCID 178432625 | 67% |
Reaction Steps
To a solution of the above-mentioned amide compound (157 mg) in benzene (4 mL) was added phosphorus pentachloride (266 mg), and the mixture was stirred at 50° C. for 3 days. After cooling to room temperature, to the reaction mixture was added 2N sodium hydroxide aqueous solution (4 ml), and the reaction mixture was stirred for an additional 30 minutes. The obtained mixture was extracted with chloroform thrice, and dried over anhydrous magnesium sulfate. The solvent was evaporated in vacuo, and the obtained residue was purified by silica gel column chromatography (C-300; hexane: ethyl acetate=1:1→1:2) to give the objective compound (100 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07482358B2 |
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| Source dataset | uspto-grants-2009_01 |
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| ORD ID | ord-f7abd373b5a948a6a02b97960fd83d02 |
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| Source note | uspto-grants-2009_01 |
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