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A) radiation. The
X-ray photo-electron spectroscopy (XPS) measurements were
performed using a Gammadata-scienta ESCA200 hemispherical
analyzer equipped with an Al (Ka 1486.6 eV) X-ray source. The
ICP analyses were carried out by a PerkineElmer optima 7300 DV
spectrometer. GC analyses were performed using a Shimadzu GC-
16A gas chromatograph equipped with a ame ionization detec-
tor and a 2 m column packed with silicon DC-200 or Carbowax
20m. The transmission electron microscopy (TEM) was carried out
on a Philips CM10 instrument operating at 100 kV. The crystal size
and microscopic morphological features were obtained on a Hitachi
S-4700 eld emission-scanning electron microscope (FE-SEM).
General procedure for SuzukieMiyaura cross-coupling reaction
catalyzed by Pd/UiO-66-NH
2
Typically, a mixture of aryl halide (1 mmol), phenylboronic acid
(1.1 mmol), K
2
CO
3
(1.5 mmol) and the Pd/UiO-66-NH
2
catalyst
(10 mg, 0.25 mol%) in a 2:1 solution of DMF/H
2
O (3 mL) was stirred
at 60
C under air atmosphere. The reaction progress was moni-
tored by GC. After completion of the reaction, the catalyst was
separated by centrifugation and the products were extracted with
ethyl acetate (3 10 mL) and. The organic phase was washed with
water (2 10 mL), dried over anhydrous Na
2
SO
4
and evaporated.
The residue was recrystallized from ethyl acetate and ether (1:3) to
afford the pure product.
Catalyst recovery and reuse
In the recyclability experiment, the reaction of 4-iodoanisole
and phenylboronic acid was chosen as model reaction. At the end
of each reaction, the catalyst was recovered by centrifugation,
washed with water and DMF, respectively, and dried at 60
C under
vacuum and used with fresh 4-iodoanisole and phenylboronic acid.
Fig. 6. The XPS spectrum of: (a) Pd/UiO-66-NH
2
showing Pd 3d
5/2
and Pd 3d
3/2
binding
energies, (b) the elemental survey scan of Pd/UiO-66-NH
2
.
Table 1
Optimization of reaction conditions in the SuzukieMiyaura cross-coupling of 4-iodoanisole (Ia) with phenylboronic acid (PBA) catalyzed by Pd/UiO-66-NH
2
.
Entry Base Ia:PBA:base [mmol] Solvent
a
Catalyst amount (mol%) T (