Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | HCID 178425474 | HCID 178425474 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86657561 | HCID 86657561 | 74.8% |
Reaction Steps
To the 500 mL round-bottomed flask with 3,4-dimethyl-1-(6-methylpyridin-2-yl)-1H-pyrazol-5-ol (6.68 g, 33 mmol) were added Et3N (5.5 mL, 39 mmol) and 35 mL CH2Cl2. the solution was cooled in dry ice acetone bath. Tf2O (6.1 mL, 36 mmol) was added slowly. The mixture was stirred at −78° C. and allowed to warm to room temperature. The mixture was then concentrated in vacuo. The crude product was purified using a Biotage Horizon System (0 to 25% EtOAc/hexane) to afford a colorless oil (8.28 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09090625B2 |
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| Source dataset | uspto-grants-2015_07 |
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| ORD ID | ord-adbb43e2726c41599ce758ac76c54987 |
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| Source note | uspto-grants-2015_07 |
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