反应详情

To 11.3 g (0.05 mol) 9,9-dihydroxymethylfluorene was added 50 ml tetrahydrofuran, then added 12.1 ml (0.15 mol) pyridine with stirring. To the resulting homogenous mixture was slowly added 14.5 ml (0.125 mol) benzoyl chloride. The mixture was stirred at room temperature for 1 hour, and then heated refluxing for 4 hours. Upon reaction completion, 70 ml water was added to dissolve the resulting salt. The mixture was extracted with toluene. The organic phase was separated, washed with saturated saline for two times, dried over anhydrous sodium sulfate. The solvent was removed to give a white solid. Recrystallization from ethyl acetate gave 9,9-bis(benzoyloxymethyl)fluorene as a white crystal, the yield was 89%, and m.p. was 144-146° C. 1HNMR: δ (ppm) 4.74(s, 4H, CH2), 7.25-7.75(m, 18H, ArH)

1. stirringThe mixture was stirred at room temperature for 1 hour
2. temperatureheated
3. temperaturerefluxing for 4 hours
4. additionwas added
5. dissolutionto dissolve the resulting salt
6. extractionThe mixture was extracted with toluene
7. customThe organic phase was separated
8. washwashed with saturated saline for two times
9. dry with materialdried over anhydrous sodium sulfate
10. customThe solvent was removed
11. customto give a white solid
12. customRecrystallization from ethyl acetate