反应详情

50.4 g (0.223 mol) of 9-hydroxy-9-fluorenecarboxylic acid are dissolved in 500 mL of methanol, combined with 5 mL (0.089 mol) of concentrated sulfuric acid and refluxed for 1 hour. After cooling, 100 mL of sodium hydrogen carbonate solution (about pH 8) are added and the methanol is largely evaporated down. The mixture is extracted with dichloromethane and water, the organic phase is dried and evaporated to dryness. The product is purified by recrystallization from ethyl acetate. Yield: 50.0 g of white crystals (93% of theoretical yield).

1. temperaturerefluxed for 1 hour
2. temperatureAfter cooling
3. customthe methanol is largely evaporated down
4. extractionThe mixture is extracted with dichloromethane and water
5. customthe organic phase is dried
6. customevaporated to dryness
7. customThe product is purified by recrystallization from ethyl acetate