Lee et al.
Synthesis of a New Conjugated Polymer Composed of Pyrene and Bithiophene Units for Organic Solar Cells
product was purified by flash silica gel chromatography
using n-hexane as an eluent. The product yield was 56%.
1H-NMR (400 MHz, CDCl3) ꢃ 0.85 (t, 3H), 1.25 (m, 6H),
1.62 (m, 2H), 2.75 (t, 2H), 6.90 (d, 2H), 7.15 (d, 1H).
(m, 8H), 1.26 (m, 4H), 1.30 (m, 24H), 1.48 (m, 4H), 2.45
(t, 4H), 7.50 (s, 2H).
2.4.5. Synthesis of an Alternating Copolymer Composed
of 3,3ꢁ-dihexylbithiophene and Pyrene
[Poly(DHBT-alt-PYR)]
2.4.2. Synthesis of 2-bromo-3-hexylthiophene (2)
Tetrakis(triphenylphosphine)palladium (0.084 mmol)
catalyst was charged into a two-necked 50 mL round
bottom flask in a glove box. To the reactor was added
a mixture of 1,6-dibromopyrene (0.921 g, 2.588 mmol),
3,3ꢁ-dihexyl-2,2ꢁ-bithiophenyl-5,5ꢁ-di-4,4,5,5-tetramethyl-
[1,3,2]dioxaborolane (1.5 g, 2.56 mmol), 10 mL of
toluene and 10 mL of THF. 2.0 M aqueous sodium
carbonate solution (8 mL, 5 eq) with Aliquat (0.103 g)
as a phase-transfer catalyst were added to the reaction
3-Hexylthiophene (5.8 g, 34.5 mmol) was dissolved in
50 mL of THF and 50 mL of acetic acid in a 250 mL one-
necked flask with a magnetic stirrer. N-Bromosuccinimide
(NBS) (6.45 g, 36.2 mmol) was added into the solution
ꢀ
in one portion, and the solution was stirred at 0 C for
2 hours. The solution was then extracted with diethylether
and brine. The organic layer was separated and dried over
anhydrous MgSO4 and the removal of solvent gave a color-
1
less oil. The product yield was 89%. H-NMR (400 MHz,
ꢀ
mixture, the solution was stirred at 80 C for 48 hours.
CDCl3) ꢃ 0.85 (t, 3H), 1.25 (m, 6H), 1.62 (m, 2H), 2.75
The polymer was then end-capped with 2-bromothiophene
and thiophene-2-boronic acid, and stirred at 80 ꢀC for
12 hours. After the reaction was quenched with methanol,
the crude product was flash-columned on Florisil using
chloroform as an eluent. The obtained solid product was
dissolved in chloroform and precipitated in methanol three
times and finally purified by a Soxhlet extractor using
methanol as a solvent. 1H-NMR (400 MHz, CDCl3) ꢃ
0.85 (t, 6H), 1.25 (m, 8H), 1.45 (m, 4H) 1.75 (m, 4H),
2.85 (t, 4H), 7.32 (s, 2H), 8.02 (d, 2H), 8.10 (d, 2H),
(t, 2H), 6.90 (d, 1H), 7.15 (d, 1H).
2.4.3. Synthesis of 3,3ꢁ-dihexyl-2,2ꢁ-bithiophene (3)
A
solution of 2-bromo-3-hexylthiophene (9.15 g,
37.2 mmol) in 40 mL dry THF was added drop-wise
manner into magnesium (2.26 g, 93.0 mmol) in 10 mL
of dry THF and the mixture was refluxed at 60 C under
ꢀ
nitrogen gas for 2 hours. Then this mixture was added
slowly into a mixture of 2-bromo-3-hexylthiophene (7.6 g,
31.0 mmol) and Ni(dppp) Cl2 (0.17 g, 0.31 mmol) in
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8.25 (d, 2H), 8.45 (d, 2H) 13C-NMR (400 MHz, CDCl3)
ꢃ 17.0, 21.5, 24.5, 25.0, 25.5, 120.5, 125.5, 126.0, 126.5,
128.0, 129.0, 129.5, 130.0, 131.0, 132.0.
IP: 86.161.220.70 On: Mon, 21 Dec 2015 10:10:28
ꢀ
30 mL of dry THF at 0 C. The mixture was refluxed
Copyright: American Scientific Publishers
ꢀ
at 60 C for 12 hours. The organic layer was extracted
with diethylether/brine three times and then was dried
over anhydrous MgSO4. Solvent was then removed under
reduced pressure, and the product was purified by frac-
tional distillation under vacuum. The product yield was
56%. H-NMR (400 MHz, CDCl3ꢄ ꢃ 0.85 (t, 6H), 1.25
(m, 12H), 1.52 (m, 4H), 2.45 (t, 4H), 6.93 (d, 2H), 7.25
(d, 2H).
3. RESULTS AND DISCUSSION
The synthesized polymer was soluble in common organic
solvents such as chloroform, chlorobenzene, toluene, etc.
and formed uniform thin film after spin-coating with the
polymer solution. The weight average molecular weights
(Mw) of poly(DHBT-alt-PYR) was determined by gel per-
meation chromatography using a polystyrene standard, and
was found to be 7,300 with polydispersity indexes of 1.70.
The polymer yield was 65% after purification. The thermal
properties of the polymers were determined with thermal
gravimetric analysis (TGA). The polymer was found to
exhibit good thermal stability, losing lessꢀthan 5% of their
weight on heating to approximately 370 C.
Figure 1 shows the UV-visible absorption and PL emis-
sion spectra of the polymer thin film. The maximum
absorption and peak emission of the polymer film was
401 and 548 nm, respectively. The UV absorption and
PL emission spectra of the polymer film was red-shifted
than those of polymer solution in chloroform (398 and
523 nm, respectively), suggesting that the effective con-
jugation would be extended in solid state due to staking
of flat pyrene and bithiophene segments. Highest occu-
pied molecular orbital (HOMO) energy level of the poly-
mer was measured by oxidation potential of polymer
1
2.4.4. Synthesis of
3,3ꢁ-dihexyl-5,5ꢁ-[di-4,4,5,5-tetramethyl-1,
3,2-dioxaborolanyl]-2,2ꢁ-bithiophene (4)
To a solution of 3,3ꢁ-dihexyl-2,2ꢁ-bithiophene (4.36 g,
13.0 mmol) in THF (60 mL) was added a 2.5 M solu-
tion of n-BuLi (17.1 mL, 27.37 mmol) in n-hexane ꢀat
ꢀ
−70 C. After 30 min, the mixture was heated to −15 C
and 2-isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane
(5.32 g, 28.6 mmol) was added. The mixture was then
heated to room temperature and stirred for 2 hours. The
reaction solution was hydrolyzed and then extracted with
diethylether and brine. Organic layer was separated, dried
over anhydrous MgSO4 and concentrated using a rotary
evaporator. The obtained crude product was purified by
flash silica gel column chromatography using a solvent
(n-hexane/ethyl acetate = 9/1). The product yield was
1
61%. H-NMR (400 MHz, CDCl3) ꢃ 0.85 (t, 6H), 1.20
J. Nanosci. Nanotechnol. 11, 4367–4372, 2011
4369