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With 5%-palladium/activated carbon; water In ethanol at 300℃; for 1h; |
1 Examples 1 to 5, Comparative Examples 1 and 2 (mixing ratio of alcohol and water)
First, in a stainless steel batch reaction tube having an inner volume of 6 cm 3,0.15 g of a powdery catalyst (5% Pd / C, manufactured by Wako Pure Chemical Industries, Ltd.) having a ratio of the mass of palladium metal to the mass of activated carbon support of 5%0.1 g of 4-propyl phenol,And ethanol and water shown in Table 1 were charged, and the air in the reaction tube was replaced with argon. Next, this reaction tube was heated to 300 ° C. using a sand bath, reacted for 1 hour, and then cooled with water.Then, the volume of the gas product was measured using a syringe,And analyzed by gas chromatography (GC-TCD).In addition, reactants and products in the solution in the reaction tube were analyzed by gas chromatography (GC-FID). As a result, in Examples 1 to 5, it was confirmed that 4-propylcyclohexanone, cis-4-propylcyclohexanol and trans-4-propylcyclohexanol, which are products resulting from the nuclear hydrogenation reaction of 4-propylphenol, It was obtained in the amount described in Table 1. On the other hand, in Comparative Example 1 and Comparative Example 2, 4-propylcyclohexanone, cis-4-propylcyclohexanol, and trans-4-propylcyclohexanol could not be obtained.In Comparative Example 2, hydrogen gas was obtained in the amount shown in Table 1.As shown in Table 1, 4-propylcyclohexanone, the product of the nuclear hydrogenation reaction of 4-propylphenol, was the most obtained in Example 1 in which the ratio of the volume of ethanol to the volume of water was 0.5 .The amount of hydrogen produced increased with increasing amount of ethanol.From Comparative Examples 1 and 2, it was also found that both ethanol and water are required for nuclear hydrogenation. |
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In ethanol; water at 299.84℃; for 1h; |
Hydrogenation of 4-propylphenol was conducted in a 316stainless steel tube reactor having an internal volume of 6.0cm3.15,16 Supported palladium catalyst (0.15 g), 4-propylphenol(0.74mmol), water (2 mL), and ethanol (1 mL) were loaded intothe reactor. The reactor was thoroughly purged with argon gasten times for the removal of any residual air. Then the reactorwas submerged into a sand bath (ACRAFT, model AT-1B) andwas maintained at 573 K. After one hour of reaction time, thereactor was taken out from the sand bath and submerged in awater bath for rapid cooling to room temperature. Gaseousproducts were collected by a syringe through sampling loopsattached to a gas chromatograph with a thermal conductivitydetector (GC-TCD) (SHIMADZU, model GC-8A). After samplingthe gaseous products, the slurry was filtered to remove thepowder catalyst and the clear liquid fraction was recovered withtetrahydrofuran (THF). The products dissolved in THF wereanalyzed using a gas chromatograph with a flame ionizationdetector (GC-FID) (SHIMADZU, model GC-14B) and a gaschromatograph with a mass spectrometer (GC-MS) (AgilentTechnologies, model HP-7890) with a DB-WAX capillarycolumn. |
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