(0.086 mmol) were suspended in 1 mL of dichloromethane, and
0.129 mmol of the diazo compound [ethyl diazoacetate (EDA) or
ethyl 2-phenyldiazoacetate (PhEDA)] in 1 mL of dichloro-
methane was added either in one portion before starting the
reaction or slowly in a dropwise manner with a syringe pump
over 2 h. Gas evolution was observed along with a smooth
change in color. The resulting mixture was stirred at ambient
temperature for 24 h. The reaction was monitored by gas chro-
matography on HP5890 II GC-MS and Konik HRGC 4000B
GC-MS chromatographs with a cross-linked (95%)-dimethyl-
(5%)-diphenylpolysiloxane (Teknokroma TRB-5MS) column of
30 meters of length; helium as a carrier gas. 20 psi; injector
temperature: 230 ꢁC; detector temperature: 250 ꢁC; oven
program for styrene: 70 ꢁC (3 min), 15 ꢁC minꢀ1 to 200 ꢁC
(5 min); retention times: ethyl diazoacetate 3.20 min, styrene
3.82 min, n-decane 5.47 min (internal reference), diethyl maleate
7.84 min, diethyl fumarate 8.02 min, cis-cyclopropanes
10.91 min, trans-cyclopropanes 11.41 min.
Acknowledgements
The financial support provided by the Spanish Ministerio de
ꢀ
Ciencia
e
Innovacion (MICINN) (Projects: Consolider
MAT2011-29020-C02-02 and
CDS2009-050-Multicat,
MAT2010-20668) is gratefully acknowledged. We thank Cristina
Guerrero for the BET measurements.
Notes and references
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4. Conclusions
We have described the use of polymer organic frameworks (Th-
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ꢀ
ꢀ
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This journal is ª The Royal Society of Chemistry 2012
J. Mater. Chem., 2012, 22, 24637–24643 | 24643