A RECYCLABLE HETEROGENEOUS PALLADIUM CATALYST
1949
analyzer at –196°C. Prior to the measurement, a sample
REFERENCES
was degassed at 50°C under reduced pressure for 12 h.
Thermogravimetric analysis was carried out in the
range 25–600°C on a Scinco S-1000TGA system under
nitrogen flow at a heating rate of 10.0 deg/min. The
FT-IR spectra were obtained on a Thermo Scientific
Nicolet iS10 FTIR spectrometer at ambient temperature.
The H NMR spectra were recorded on a Varian Unity
Inova instrument at 400 MHz from solutions prepared
by digesting 10 mg of a sample in a mixture of
1
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3
5% DCl in D O). The metal content of the catalyst
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2
was determined by inductively coupled plasma mass
spectrometry using a Perkin Elmer Elan 6100 ICP/MS
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data were obtained using a Bruker 3800 GC/1200L MS
instrument.
Synthesis of MOF3. An equimolar mixture of
MOF2 [18] and Pd(OAc) in acetone was kept for 10 h
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2
at room temperature. Prior to drying, the solvated
catalyst was soaked in chloroform for three days, and
the solvent was changed every 24 h during this process.
Hydrogenation of styrene oxide. A small vial was
charged with MOF3 (11 mg, 2 mol %), 1 mL of metha-
nol was added, and styrene oxide (0.4 mmol) was then
added. The vial was capped with a rubber stopper, and
the mixture was stirred at room temperature in a hydro-
gen atmosphere at ambient pressure using a hydrogen-
filled balloon. After completion of the reaction (5 h),
the mixture was centrifuged, and the supernatant solu-
tion was separated for analysis.
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Catalyst recycling. After completion of the reac-
tion, the mixture was centrifuged, and the solution
containing product was decanted. The catalyst was
washed with methanol (2×2 mL), separated by centri-
fugation, and dried at 50°C for the next run.
1
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This study was performed under financial support by
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Technology.
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1
1
CONFLICT OF INTERESTS
The authors declare the absence of conflict of interests.
RUSSIAN JOURNAL OF ORGANIC CHEMISTRY Vol. 55 No. 12 2019