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Macromolecules, Vol. 35, No. 9, 2002
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(d, J ) 8.5 Hz, 4 H), 7.06 (d, J ) 8.5 Hz, 4 H), 4.83 (s, 2 H),
4.71 (br, 4 H), 3.54-3.51 (m, 2 H), 3.50-3.39 (m, 2 H), 2.97 (s,
4 H), 1.66-1.60 (m, 4 H), 1.52 (t, J ) 3.1 Hz, 6 H), 1.40-1.25
(m, 12 H). 13C NMR (CDCl3): δ 207.2, 170.7, 149.6, 138.7,
127.4, 120.9, 99.2, 82.1, 74.7, 68.8, 29.7, 29.5, 29.4, 29.3, 26.3,
13.0.
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Cr oss-Lin k in g of P olyeth er Obta in ed fr om 1a , 2a , a n d
4b w ith BF 3OEt2. A round-bottomed flask equipped with a
three-way stopcock was purged with argon. A solution of the
polymer from 1a , 2a , and 4b (0.096 g, 0.25 mmol) in CH2Cl2
(0.35 mL) was added to the flask. After the solution was cooled
to -50 °C, a solution of BF3OEt2 (3 µL, 0.025 mmol) in CH2-
Cl2 (0.25 mL) was added at -50 °C via a syringe, and the
solution was warmed to room temperature and stirred for 90
min. The resultant gel was washed with CH2Cl2 in a Soxhlet
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.
4724.
Cr oss-Lin k in g of P olyeth er Obta in ed fr om 1a , 2a , a n d
4b w ith DP SP . A solution of polymer from 1a , 2a , and 4b
(0.096 g, 0.25 mmol) and DPSP (0.056 g, 0.065 mmol) in CHCl3
(0.25 mL) was placed on aluminum foil, followed by evapora-
tion of CHCl3, and UV irradiation of the polymer. After
predetermined intervals, IR spectra were measured for deter-
mination of the conversion of allenyl groups by comparison
with absorption areas between allenyl groups at 1958 cm-1
and terminal methylene at 1719 cm-1. After 80 min, the
conversion of allenyl groups reached 60%, and the cross-linked
polymer was obtained as a brownish glassy plate. IR (neat):
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2930, 2855, 1958, 1720, 1102, 845, 795, 710 cm-1
.
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Ack n ow led gm en t. We gratefully thanks Professor
Nishikubo at Kanagawa University for a generous gift
of DPSP and use of BIO-RAD RT/IR.
Refer en ces a n d Notes
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