反应详情

To a solution of 0.20 g (0.45 mM) of 2-octyl-7-(5-hexyl-1,3,4-thiadiazole-2-yl)fluorene in 20 ml of pyridine, 0.27 ml of 40%-trimethylbenzylammonium hydroxide aqueous solutions as added at 3.5°-4.5° C. under stirring on ice water bath, followed by stirring for 0.5 hour at 3.5°-4.5° C. After the reaction, the reaction mixture was poured into ice water to precipitate a crystal. The crystal was recovered by filtration, washed with water and dissolved in toluene, followed by drying with anhydrous sodium sulfate and distilling-off of the solvent under reduced pressure to obtain a residue. The residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=20/1) and recrystallized from a mixture solvent of toluene-acetone to obtain 0.11 g of 2-octyl-7-(5-hexyl-1,3,4-thiadiazole-2-yl)fluorenone (Yield: 53.3%). ##STR89##

1. stirringby stirring for 0.5 hour at 3.5°-4.5° C
2. customAfter the reaction
3. customto precipitate a crystal
4. filtrationThe crystal was recovered by filtration
5. washwashed with water
6. dissolutiondissolved in toluene
7. dry with materialby drying with anhydrous sodium sulfate and distilling-off of the solvent under reduced pressure
8. customto obtain a residue
9. customThe residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=20/1)
10. customrecrystallized from a mixture solvent of toluene-acetone