Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4,4,4-Trifluoro-N-hydroxy-2-methyl-3-oxobutyramide | HCID 10081104 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | HCID 178431795 | HCID 178431795 | 44% |
Reaction Steps
4,4,4-Trifluoro-N-hydroxy-2-methyl-3-oxobutyramide (500 mg, 2.70 mmol) was dissolved in aq. 90% H2SO4 (5.5 mL). The mixture was heated to 75° C. for 90 min, and then allowed to cool to rt. Water (15 mL) was added, and the mixture was extracted with Et2O (2×). The combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification by FC (EtOAc/heptane/AcOH 20:80:1→25:75:1→33:66:1) yielded the title compound (197 mg, 44%). TLC: Rf=0.43 (EtOAc/heptane 1:1+1% AcOH).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08138340B2 |
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| Source dataset | uspto-grants-2012_03 |
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| ORD ID | ord-1109117c8e5043e08b87392eb89d2e6f |
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| Source note | uspto-grants-2012_03 |
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