反应详情

温度

70 °C

To 6.8 g (0.03 mol) 9,9-di(hydroxymethyl)fluorene was added 4.3 ml (0.06 mol) acrylic acid and 30 ml toluene. To the resulting homogenous mixture was added 0.2 ml concentrated sulfuric acid. Then the reaction mixture was heated refluxing for 7 hours, and the water resulted in the reaction process was separated by a water separator. The mixture was cooled to 70° C., neutralized to alkalinity with saturated sodium carbonate solution, and extracted with toluene. The organic phase was washed with saturated saline to neutrality and dried over anhydrous sodium sulfate. The solvent was removed. Purification by column chromatography gave 9,9-bis(acryloyloxymethyl)fluorene as a white solid, and the yield was 35%. m.p. was 73-75° C. 1HNMR: δ (ppm) 4.48(s, 4H, OCH3), 5.85-6.43(m, 6H, H on acryl), 7.32-7.78(m, 8H, ArH)

1. temperatureThen the reaction mixture was heated
2. temperaturerefluxing for 7 hours
3. customwas separated by a water separator
4. extractionextracted with toluene
5. washThe organic phase was washed with saturated saline to neutrality
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was removed
8. customPurification by column chromatography