反应详情

To 5.64 g of Mg placed into a 1000 ml three-neck flask, 80 g of 9,9-dihexyl-2-bromofluorene in 300 ml THF was slowly added dropwise, to prepare a Grignard reagent. After a temperature of a reaction chamber was decreased to −40° C. or less, 52 g of 2,7-dibromofluorenone was added to the reaction bath in a nitrogen atmosphere. The temperature was gradually increased to room temperature, followed by stirring for 10 hours. The resulting reaction solution was poured into water, after which an extraction was performed using diethyl ether. The solvent was evaporated using a rotary evaporator. A column chromatography separation resulted in 60 g (58%) of (9-(9,9-dihexylfluoren-2-yl)-2,7-dibromofluoren-9-ol) (1).

1. customwas decreased to −40° C. or less
2. customThe resulting reaction solution
3. extractionafter which an extraction
4. customThe solvent was evaporated
5. customa rotary evaporator
6. customA column chromatography separation
7. customresulted in 60 g (58%) of (9-(9,9-dihexylfluoren-2-yl)-2,7-dibromofluoren-9-ol) (1)