反应详情

温度

100 °C

In a pressure vessel, combine 6-fluoro-pyridine-3-carbaldehyde (4 g, 32 mmol), ethylene glycol (3 g, 48 mmol), copper (II) chloride di-hydrate (0.56 g, 3.2 mmol) and THF (10 mL). Heat the mixture at 100° C. for 1 hour. Dilute the mixture with chloroform-isopropanol (3:1, 100 mL). Wash the organic phase with saturated aqueous sodium chloride and water. Dry the organic layer over sodium sulfate. Concentrate the solution in vacuo to brown oil. Purify by column chromatography (20% ethyl acetate in hexane) to afford the title compound (2.1 g, 39%) as a pale yellow oil. MS (ES) m/z 170 [M+1]+.

1. customIn a pressure vessel, combine
2. washWash the organic phase with saturated aqueous sodium chloride and water
3. dry with materialDry the organic layer over sodium sulfate
4. concentrationConcentrate the solution in vacuo to brown oil
5. customPurify by column chromatography (20% ethyl acetate in hexane)