Table 2 Stepwise Stille polymerization with the optimization data

From: Stepwise heating in Stille polycondensation toward no batch-to-batch variations in polymer solar cell performance

Entry

Solvent (Conc.)

Catalyst (mol%)

Mn (kDa)a

Mw (kDa)a

Ð a

Yield (%)b

11

Toluene:DMF (0.05 M)

Pd(PPh3)4 (4.0)

67.2

90.1

1.34

-c

12d

Toluene:DMF (0.05 M)

Pd(PPh3)4 (4.0)

43.9

82.6

1.88

-c

13d

Toluene:DMF (0.05 M)

Pd(PPh3)4 (4.0)

42.5

99.8

2.35

-c

14

Toluene:DMF (0.10 M)

Pd(PPh3)4 (4.0)

31.3

65.1

2.08

63

15

Toluene:DMF (0.026 M)

Pd(PPh3)4 (4.0)

82.1

125

1.52

65

16

Toluene:DMF (0.026 M)

Pd(PPh3)4 (3.0)

110

151

1.37

81

17

Toluene:DMF (0.026 M)

Pd(PPh3)4 (2.0)

151

195

1.29

79

18

Toluene:DMF (0.026 M)

Pd(PPh3)4 (1.0)

184

223

1.21

85

19e

Conventional polymerization

Pd(PPh3)4 (1.0)

46.9

75.8

1.62

 72

  1. The stepwise Stille polycondensation was carried out under an argon atmosphere in a long Schlenk tube of monomer 1, 2, and Pd(PPh3)4, and procedures included the initial heating at 120 °C for 1 h, the cooling step at 60 °C for 11 h, and the final heating at 120 °C for 1 day
  2. a Mn, Mw, and Ð values were determined from GPC measurement using 1,2,4-trichlorobenzene at 120 °C calibrated with polystyrene as standard
  3. b Yields were estimated from the amounts of the chloroform fractions
  4. c Each fraction was extracted by a syringe, then precipitated in methanol with Soxhlet purification for only GPC analysis
  5. d The cooling temperature was investigated at 80 and 100 °C for entries 12 and 13, respectively
  6. e 1.0 mol% Pd catalyst was employed for conventional Stille polymerization. A mixture of monomer 1, 2, and Pd(PPh3)4 in a binary solvent of toluene and DMF (4:1 vol%, 0.026 M) was reacted at 120 °C for 1 day in a long Schlenk tube under an argon condition
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