10.1002/ejic.201700993
European Journal of Inorganic Chemistry
FULL PAPER
observations were performed with
a
JEOL JEM-1400 transmission
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electron microscopy (TEM) system operating at 120 kV. ICP analyses
were conducted by ICP AES (SPS 7800, Seiko Instruments). 1H NMR
spectra were recorded on a JEOL JNM-A500 spectrometer. The 1HNMR
chemical shifts are referenced to the residual internal benzene-d6.
Synthesis of MIL-101(SO3H)
Monosodium 2-sulfoterephthalic acid (3.35 g, 12.5 mmol), CrO3
(1.25 g, 12.5 mmol) and concentrated aqueous hydrochloric acid (0.91 g
(12 N), 25 mmol) were dissolved in water (50 ml), then transferred to
Teflon-lined stainless steel autoclave. The resulting solution was heated
at 453 K for 6 days under hydrothermal conditions. The reaction product
was finally obtained after washing three times with 100 ml of DMF under
sonication and subsequently drying in vacuo at 120 oC for 2 hrs.
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Synthesis of 1
To RhCl(PPh3)3 (92.52 mg, 0.1 mmol) in 7.5 ml of CH3CN, was
added MIL-101(SO3H) (50 mg) under Ar and the resulting solution was
o
heated at 80 C for 12 hrs. After filtration, thorough washing with soxhlet
apparatus for 12 hrs with CH3CN and drying in vacuo at 120 oC for 2 hrs,
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brown powder of 1 was obtained.
Hydrogenation reaction of alkene substrates with H2 gas
In a typical procedure, 1 (2.0 mg, 0.03 mol% [Rh]) and 1-octene (0.5
ml, 3.2 mmol) were put into benzene-d6. The resulting suspension was
transferred to pressurized vessel and then started the reaction at 70 oC
after introducing H2 gas inside the vessel. The reaction yield was finally
checked by 1HNMR after the reaction.
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This research was carried out with support from JSPS KAKENHI
(Grant 15K17836).
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Keywords: hydrogenation • metal-organic frameworks •
heterogeneous catalysis • microporous materials • rhodium
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