反应条件: temp:105.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: In an inert atmosphere, the compound A (0.55 g), the compound B (0.61 g), (triphenylphosphine)palladium (0.01 g), methyltrioctylammonium chloride (manufactured by Aldrich Co.; trade name: Aliquat 336 (registered trademark)) (0.20 g), and toluene (10 mL) were mixed, and the resultant reaction mixture was heated to 105° C. Into the reaction solution, a 2 mol/L sodium carbonate aqueous solution (6 mL) was added dropwise, and the resultant reaction mixture was refluxed for 8 hours. To the reaction solution, 4-tert-butylphenylboronic acid (0.01 g) was added, and the resultant reaction mixture was refluxed for 6 hours. Next, to the reaction mixture, a sodium diethyldithiocarbamate aqueous solution (10 mL, concentration: 0.05 g/mL) was added, and the resultant reaction mixture was stirred for 2 hours. The resultant solution mixture was added dropwise into 300 mL of methanol, and the resultant reaction mixture was stirred for 1 hour. Then, a deposited precipitate was filtered and the precipitate was dried under reduced pressure for 2 hours, followed by dissolving the precipitate in 20 mL of tetrahydrofuran. The resultant reaction solution was added dropwise into a solvent mixture of 120 mL of methanol and 50 mL of a 3% by weight acetic acid aqueous solution, and the resultant reaction mixture was stirred for 1 hour. A deposited precipitate was filtered, and the precipitate was dissolved in 20 mL of tetrahydrofuran. The thus obtained reaction solution was added dropwise into 200 mL of methanol, and the resultant reaction mixture was stirred for 30 minutes. A deposited precipitate was filtered to obtain a solid. The obtained solid was dissolved in tetrahydrofuran, and the resultant solution was passed through an alumina column and a silica gel column to purify the solution. The tetrahydrofuran solution recovered from the column was concentrated, and the concentrate was added dropwise into methanol (200 mL), followed by filtering and drying a deposited solid. The yield of obtained poly[9,9-bis[3-ethoxycarbonyl-4-bis[2-[2-(2-methoxyethoxy)ethoxy]ethoxy]phenyl]-fluorene] (polymer A (BSAFEGP)) was 520 mg.
the resultant reaction mixture
the resultant reaction mixture
was refluxed for 8 hours
the resultant reaction mixture
was refluxed for 6 hours
the resultant reaction mixture
the resultant reaction mixture
was stirred for 1 hour
Then, a deposited precipitate was filtered
the precipitate was dried under reduced pressure for 2 hours
by dissolving the precipitate in 20 mL of tetrahydrofuran
The resultant reaction solution
the resultant reaction mixture
was stirred for 1 hour
A deposited precipitate was filtered
the precipitate was dissolved in 20 mL of tetrahydrofuran
The thus obtained reaction solution
the resultant reaction mixture
was stirred for 30 minutes
A deposited precipitate was filtered
to obtain a solid
a silica gel column to purify the solution
The tetrahydrofuran solution recovered from the column
was concentrated
the concentrate was added dropwise into methanol (200 mL)
by filtering
drying a deposited solid
来源 ID: ord-f8f9145c562b41d6ba22f210a09c72ba