The novel monovinyl-functional silsesquioxane cage
1-(9-decenyl)-3,5,7,9,11,13,15-heptaethylpentacyclo[9.5.1.13,9.15,15.17,13]octasiloxane
has been prepared and copolymerized with ethene
and propene. The monovinyl-functional spherosiloxane was obtained
from the octahydridosilsesquioxane
(HSiO3/
2)8 via hydrosilation with
dibrominated decadiene, followed by reaction of the nonreacted
SiH
groups with ethene, debromination, and chromatographic separation.
Homopolymerization and copolymerization with ethene and propene was performed using different
methylalumoxane-activated
metallocene catalysts. Depending on catalyst structure comonomer
incorporation between 17 and 25 wt
% was achieved. High molar mass copolymers were obtained
containing pendant octasiloxane cubes.
Characterization by 13C, 1H, and
29Si NMR spectroscopy confirmed that the catalyst did
not modify the
Si−O−Si framework. Incorporation up to 25 wt % (1.2 mol %)
of the spherosiloxane-based monomer
accounted for a decrease of the melting temperature by 18 K with
respect to polyethene. As demonstrated
by means of thermal gravimetric analysis, thermostability under air was
improved in the polyethene
copolymer in comparison to polyethene.
EUS-TNB allows reliable tissue sampling for the diagnosis of pancreatic masses, but its use is limited to lesions in the body and tail of the pancreas. EUS-FNAB using a 22-gauge needle may be useful for accurate diagnosis in some patients with masses in the uncinate process or the head of the pancreas.
The homologous series of 8-fold alkyl-substituted
octasilsesquioxane has been prepared
by hydrosilation of alkenes with octakis(hydridosilsesquioxane)
(HSiO3/2)8. Ethene,
propene,
1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1-nonene, and
1-decene were employed
either in bulk or in toluene solution. The homologous series of
1,3,5,7,9,11,13,15-octaalkylpentacyclo[9.5.1.13,9.15,15.17,13]octasiloxanes,
which are interesting model compounds
for silsesquioxane-based materials was characterized by 1H,
13C, and 29Si NMR
spectroscopy,
IR and mass spectroscopy, and elemental analysis. Melting points
of the compounds were
studied by DSC, revealing a strong decrease of the melting point from
the octapropyl-substituted T8 to the octapentyl derivative. Melting
points for derivatives with longer n-alkyl
chains showed an odd−even effect. TGA evidenced thermal
stability under nitrogen up to
temperatures between 200 and 400 °C and under air up to temperatures
between 200 and
250 °C.
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