Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 68514586 | HCID 68514586 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68516097 | HCID 68516097 | 17.9% |
Reaction Steps
To a solution of N-[2-({[(2-chloroethyl)amino]carbonyl}amino)ethyl]-5-(5-fluoropentyl)-1-(4-{[(2,2,2-trifluoroethyl)amino]carbonyl}phenyl)-1H-1,2,3-triazole-4-carboxamide (0.06 g) obtained in Example 301 in THF (5.5 ml) was added potassium tert-butoxide (0.03 g), and the mixture was stirred at room temperature overnight. The reaction mixture was neutralized with 1N hydrochloric acid, and the solvent was evaporated under reduced pressure. Water was added to the obtained residue, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by preparative HPLC (acetonitrile-water) and recrystallized from acetonitrile-water to give the title compound as a white powder (0.01 g, 14%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07803822B2 |
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| Source dataset | uspto-grants-2010_09 |
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| ORD ID | ord-4b8d3e6ac800457a9bf98baff954b78d |
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| Source note | uspto-grants-2010_09 |
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