Supplementary Information - Royal Society of Chemistry

Electronic Supplementary Material (ESI) for Polymer Chemistry.
This journal is © The Royal Society of Chemistry 2014
Supplementary Information for
The Pd(AcO)2/t-Bu3P/K3PO4 catalytic system for the control of
the Suzuki cross-coupling polymerisation
by
Roberto Grisorio, Piero Mastrorilli and Gian Paolo Suranna
DICATECh - Dipartimento di Ingegneria Civile, Ambientale, del Territorio, Edile e di Chimica del
Politecnico di Bari, via Orabona, 4 I-70125 Bari, Italy
1
Figure S1. 1H-NMR spectrum of 2,7-diphenyl-9,9-di-n-octylfluorene.
2
Figure S2. 13C{1H}-NMR spectrum of 2,7-diphenyl-9,9-di-n-octylfluorene.
3
4000
Intensity (a.u.)
3000
2000
1000
0
360
370
380
390
400
410
420
m/z
Figure S3. HRMS(+) spectrogram of the reaction mixture obtained according to Method A (1 equiv t-Bu3P)
showing complex  as Na-adduct.
12000
Intensity (a.u.)
10000
8000
6000
4000
2000
0
490
495
500
505
510
515
520
525
530
m/z
Figure S4. HRMS(+) spectrogram of the reaction mixture obtained according to Method A (2 equiv t-Bu3P)
showing complex  as [M – AcO]+.
4
Figure S5. Typical 1H-NMR spectrum of the poly(9,9-di-n-octylfluorene)s obtained by method B.
5
Figure S6. HRMS(+) spectrogram of the products obtained according to Method B with a FL/Pd(AcO)2
molar ratio of 2/1.
6
Figure S7. 1H-NMR spectrum (aromatic region) of the polymer isolated from entry 12.
7
Figure S8. 1H-NMR spectrum (aromatic region) of the polymer isolated from entry 13.
Figure S9. 1H-NMR spectrum (aromatic region) of the polymer isolated from entry 14.
8
entry 12 (27000 Da)
entry 13 (17900 Da)
entry 14 (10000 Da)
5,0
5,5
6,0
6,5
7,0
7,5
8,0
8,5
9,0
Elution time (min)
Figure S10. GPC traces of the isolated polymers (Table 1 of the manuscript, entries 12-14).
35000
30000
Mn (Da)
25000
20000
15000
10000
5000
0
5
10
15
20
25
Monomer/Pd(AcO)2
Figure S11. Number-average molecular weights (Mn) vs monomer/Pd(AcO)2 feed ratio of the isolated
polymers (Table 1 of the manuscript, entries 12-14).
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