反应详情

In a 30 ml-round-bottomed flask, 0.65 g (1.45 mM) of N-heptanoyl-N'-(7-octyl-2-fluorenecarbonyl)hydrazine, 0.62 g (1.53 mM) of Lawesson's reagent and 10 ml of tetrahydrofuran were placed, followed by heat-refluxing for 1.5 hours. After the reaction, the reaction mixture was poured into a solution of 0.45 g of sodium hydroxide in 100 ml of ice water to precipitate a crystal. The crystal was recovered by filtration, washed with water and dissolved in toluene, followed by washing with water, drying with anhydrous sodium sulfate and distilling-off of the solvent. The residue was purified by silica gel column chromatography (eluent: toluene) and recrystallized two times from a mixture solvent of toluene-methanol to obtain 0.40 g of 2-octyl-7-(5-hexyl-1,3,4-thiadiazole-2-yl)fluorene (Yield: 61.8%). ##STR87##

1. temperatureby heat-refluxing for 1.5 hours
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. washby washing with water
8. dry with materialdrying with anhydrous sodium sulfate and distilling-off of the solvent
9. customThe residue was purified by silica gel column chromatography (eluent: toluene)
10. customrecrystallized two times from a mixture solvent of toluene-methanol