反应详情

2-(Hydroxyimino)-3-(4-phenylthiophen-2-yl)propanoic acid (0.8 g, 3.1 mmol) was heated in acetic anhydride (5 mL) for 1.5 h. The reaction mixture was cooled to room temperature and treated with water. The product was extracted with EtOAc and the organic layer was washed with H2O and brine, dried over anhydrous Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel 60-120 mesh, eluent 10-15% EtOAc in petroleum ether) to afford 2-(4-phenylthiophen-2-yl)acetonitrile (0.45 g, yield 73%) as a pale yellow solid. 1H NMR (400 MHz, CDCl3) δ 7.57-7.53 (m, 2H), 7.43-7.39 (m, 2H), 7.37-7.36 (m, 2H), 7.34-7.30 (m, 1H), 3.96 (s, 2H).

1. extractionThe product was extracted with EtOAc
2. washthe organic layer was washed with H2O and brine
3. dry with materialdried over anhydrous Na2SO4
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by column chromatography (silica gel 60-120 mesh, eluent 10-15% EtOAc in petroleum ether)