反应详情

温度

75 °C

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).

1. temperatureto cool to rt
2. extractionthe mixture was extracted with Et2O (2×)
3. dry with materialextracts were dried over MgSO4
4. filtrationfiltered
5. customthe solvents were removed under reduced pressure
6. customPurification by FC (EtOAc/heptane/AcOH 20:80:1→25:75:1→33:66:1)