反应详情

Potassium carbonate (3.1 g, 22 mmol) was added to a solution of 2-(2-Fluoro-4-hydroxy-phenyl)-2-methyl-propionitrile (1.0 g, 6.0 mmol) and 2-Chloro-1-cyclopentyl-ethanone (3.3 g, 22 mmol) in DMF (20 mL). The mixture was stirred at room temperature for 16 hours. The mixture was poured into water (100 mL) and extracted with EtOAc (2×50 mL). The organics were washed with brine (100 mL), dried over Na2SO4, filtered and concentrated. The residue was purified by flash column chromatography (0–15% EtOAc in hexanes) to give the product (1.2 g, 75% yield) as a clear oil. 1H NMR (300 MHz, CDCl3) δ: 1.57–1.93 (m, 14 H), 3.10 (m, 1 H), 4.64 (s, 2 H), 6.65 (d, J=9.6 Hz, 2 H), 7.37 (t, J=8.9 Hz, 1 H).

1. extractionextracted with EtOAc (2×50 mL)
2. washThe organics were washed with brine (100 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by flash column chromatography (0–15% EtOAc in hexanes)