反应详情

The 5-ethoxy-2-fluoro-4-hydroxy-benzaldehyde (9.15 g) described in example 1.3 was dissolved in toluene (80 ml). Ethylene carbonate (5.25 g) and tetrabutylammonium iodide (1.83 g) were added and the mixture was heated to reflux for 22 h. The mixture was cooled to room temperature and filtered over a plug of silica gel. The product was eluted with hexane/ethyl acetate. The solvent was evaporated and the solid was washed with hot hexane to give 10.3 g of 5-ethoxy-2-fluoro-4-(2-hydroxy-ethoxy)-benzaldehyde as a slightly orange solid. MS: 228 ([M]+).

1. temperaturethe mixture was heated
2. temperatureto reflux for 22 h
3. filtrationfiltered over a plug of silica gel
4. washThe product was eluted with hexane/ethyl acetate
5. customThe solvent was evaporated
6. washthe solid was washed with hot hexane