反应详情

温度

65 °C

To a mixture of 1-(4-chloro-3-fluorophenyl)-2-methylpropan-2-ol (8.61 g, 42.50 mmol), acetonitrile (13 mL, 255.0 mmol) and acetic acid (80 mL) was added sulfuric acid (13 mL) dropwise and the mixture was heated at 65° C. for 5 h. The mixture was cooled to rt and poured into ice water (400 mL) and the resulting mixture was adjusted to pH>11 with NaOH, and extracted with EtOAc (150 mL×3). The combined organic phases were washed with brine (150 mL×2), dried over anhydrous Na2SO4 (40 g) and filtered. The filtrate was concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=2:1) to give the title compound as a yellow solid (4.38 g, 42.1%). The compound was characterized by the following spectroscopic data:

1. temperatureThe mixture was cooled to rt
2. extractionextracted with EtOAc (150 mL×3)
3. washThe combined organic phases were washed with brine (150 mL×2)
4. dry with materialdried over anhydrous Na2SO4 (40 g)
5. filtrationfiltered
6. concentrationThe filtrate was concentrated in vacuo
7. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=2:1)