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DH5a:
0.50 g (1.41 mmol) of DH5, 4.7 mL of THF (conc.
0.3 M), 14 µL of a 1 M solution of TBAF, gel after 15 min,
orange powder, 0.45 g (100%). FT IR (KBr) ν (cm–1): 1080,
1152, 1265 3620. 29Si CP-MAS NMR δ (ppm): –25, –31.
SBET (m2 g–1): 157.
Catalytic polycondensation of DM1, DM3, and DM5
(sol–gel route)
General procedure
A solution in THF of 1 mol% of the catalyst TBAF and
water was added to a solution of the precursor DM in THF
at room temperature. After various reaction times a gel or a
precipitate formed, which was treated as above leading to a
powder. The FT IR and 13C CP-MAS NMR data were the
same as those of the corresponding solids obtained by the
thermal route, an additional signal at δ = 50 ppm owing to
residual methoxy groups was present in all cases.
DM1a:
2.13 g (7.44 mmol) of DM1, 7.10 mL of THF (conc.
1 M), 74.4 µL of a 1 M solution of TBAF, 270 µL of water,
gel after 5 min, white powder (1.48 g, 103%). 29Si CP-MAS
NMR δ (ppm): –15, –24, –33. SBET (m2 g–1): 1000.
DM3a:
0.54 g (1.39 mmol) of DM3, 4.7 mL of THF (conc.
0.3 M), 14 µL of a 1 M solution of TBAF, 50 µL of water,
gel after 15 min, white powder (0.45 g, 109%). 29Si CP-
MAS NMR δ (ppm): –25, –31. SBET (m2 g–1): 450.
DM5a:
0.75 g (1.83 mmol) of DM5, 6.1 mL of THF (conc.
0.5 M), 18 µL of a 1 M solution of TBAF, 66 µL of water,
gel after 5 min, orange powder (0.58 g, 100%). 29Si CP-
MAS NMR δ (ppm): –25, –31. SBET (m2 g–1): 500.
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Assink, and K.J. Shea. Chem. Mater. 8, 656 (1996).
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(1994).
Acknowledgements
The authors acknowledge the Dow Corning Corporation
for supporting this research and thank Dr. Pierre Chevalier
from Dow Corning (Barry, U.K.) for fruitful discussions.
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