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Chapter 7 177<br />
7.3.2 Catalytic reactions using Ru-DEMOFs as catalysts<br />
7.3.2.1 Ethylene dimerization<br />
In a typical run (entry 5), 2.1 mg of the activated Ru-MOF 1c was put in a 10 ml steel<br />
reactor followed by adding of 0.81 ml of Et2AlCl (1M in heptane), 2.1 ml of toluene and<br />
0.09 ml of undecane (0.01 M in toluene). After degassing, the reactor was flushed with<br />
C2H4 (800psi) and placed in a pre-heated oil bath at 80 °C with stirring for 2 hours.<br />
Subsequently, the reaction was stopped and the reactor was cooled down at -7 °C in a<br />
mixture of dry ice and ethylene glycol bath. Cold distilled water was added to quench the<br />
reaction. The organic layer kept cold was then quickly analyzed by gas chromatography<br />
(SRI 8610V GC, 60 m x 0.54 mm internal diameter, 5.0 µm MXT-1 capillary columns) using<br />
undecane signal as a reference. In case of no additive, the volume of toluene was changed<br />
to 2.91 ml. Other parameters are the same as entry 5 described above.<br />
7.3.2.2 Paal-Knorr reaction<br />
In a typical run, 5 mg of the activated Ru-MOF/DEMOFs in 0.5 ml of toluene were<br />
introduced into 125 mg (1.1 mmol) of 2,5-hexadione and 95 mg (1 mmol) of aniline and<br />
were stirred at 90 °C for 24h under air. The reaction was followed by taking aliquots every<br />
hour and analyzing the products by GC-MS. The reactions were performed in closed<br />
(pressurize able) reaction vials.<br />
7.3.3 Synthesis of [Cu3(BTC)2]n (Cu-BTC)<br />
[Cu3(BTC)2]n was prepared from a reported method [35] at a litter lower temperature (120<br />
°C). Specifically, Cu(NO3)2∙3H2O (1.8 mmol, 438 mg) and 1, 3, 5-benzentricarboxylic acid<br />
(H3BTC, 1.0 mmol, 210 mg) were put into a Teflon vessel, and a solution of 12 ml H2O:EtOH<br />
(1:1) was added. The vessel was sealed in an autoclave and kept in a preheated oven at<br />
100 °C for 12 h. The crude product was filtered and washed several times with distilled<br />
water and absolute ethanol, respectively. After dried under ambient conditions the<br />
obtained powder (152 mg) was further activated by heating at 120 °C for 24 h under<br />
dynamic vacuum (ca. 10 -3 mbar).
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