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With 0.43% Pd/C; hydrogen; In water; at 170℃; for 0.0025h;Autoclave;
EXAMPLES The following experiments were conducted in a stainless steel reactor wherein a bed of solid catalyst was placed. The catalyst bed was kept at the same temperature. Feedstock containing FDCA and FFCA was fed over the bed of catalyst. The feedstock was an aqueous stream containing 0.5 percentwt of crude FDCA composition. The crude FDCA composition consisted of 98.0 percentwt of FDCA, 1.0 percentwt of FFCA, and about 1.0 percentwt of the monomethyl ester of FDCA (FDCA-ME). The composition further contained some ppm of the components of the oxidation catalyst, viz. cobalt, manganese and bromine. Hydrogen-containing gas, consisting of 10 percentvol hydrogen and 90 percentvol nitrogen, was used for the hydrogenation. The catalysts used were Catalyst 1 , comprising 5 percentwt palladium on carbon and Catalyst 2, comprising 0.43 percentwt palladium on carbon. The experiments were conducted as follows. The reactor was charged with a desired load of the desired catalyst. The bed of catalyst was vented several times with hydrogen to remove any oxygen. Unless otherwise indicated, the reactor was subsequently pressurized with the hydrogen-containing gas to a pressure of 15 bar (at 20°C) and heated to the desired reaction temperature before the feedstock was passed over the bed of catalyst with the desired space velocity, expressed as weight hourly space velocity (WHSV) in grams of feedstock per gram of catalyst per hour. The Tables may also contain the contact time or residence time. EXAMPLE 1 In order to show the influence of the reaction temperature on the conversion of the FFCA to HMFA and MFA Catalysts 1 and 2 were used in experiments wherein the above feedstock was passed over beds of the two catalysts with different space velocities and at different reaction temperatures. From the reactor effluent the amounts of FFCA, HMFA and MFA were determined. The results are shown in Table 1. The amounts of FFCA, HMFA and MFA are expressed as mass percent, based on the amount of FFCA in the feedstock.
With 0.43% Pd/C; hydrogen; In water; at 160℃; for 0.0025h;Autoclave;
EXAMPLES The following experiments were conducted in a stainless steel reactor wherein a bed of solid catalyst was placed. The catalyst bed was kept at the same temperature. Feedstock containing FDCA and FFCA was fed over the bed of catalyst. The feedstock was an aqueous stream containing 0.5 percentwt of crude FDCA composition. The crude FDCA composition consisted of 98.0 percentwt of FDCA, 1.0 percentwt of FFCA, and about 1.0 percentwt of the monomethyl ester of FDCA (FDCA-ME). The composition further contained some ppm of the components of the oxidation catalyst, viz. cobalt, manganese and bromine. Hydrogen-containing gas, consisting of 10 percentvol hydrogen and 90 percentvol nitrogen, was used for the hydrogenation. The catalysts used were Catalyst 1 , comprising 5 percentwt palladium on carbon and Catalyst 2, comprising 0.43 percentwt palladium on carbon. The experiments were conducted as follows. The reactor was charged with a desired load of the desired catalyst. The bed of catalyst was vented several times with hydrogen to remove any oxygen. Unless otherwise indicated, the reactor was subsequently pressurized with the hydrogen-containing gas to a pressure of 15 bar (at 20°C) and heated to the desired reaction temperature before the feedstock was passed over the bed of catalyst with the desired space velocity, expressed as weight hourly space velocity (WHSV) in grams of feedstock per gram of catalyst per hour. The Tables may also contain the contact time or residence time. EXAMPLE 1 In order to show the influence of the reaction temperature on the conversion of the FFCA to HMFA and MFA Catalysts 1 and 2 were used in experiments wherein the above feedstock was passed over beds of the two catalysts with different space velocities and at different reaction temperatures. From the reactor effluent the amounts of FFCA, HMFA and MFA were determined. The results are shown in Table 1. The amounts of FFCA, HMFA and MFA are expressed as mass percent, based on the amount of FFCA in the feedstock.
With hydrogen; In 1,4-dioxane; water; under 41254.1 Torr;Heating; Sealed tube;
[0192] 20 mg of different powder catalyst were placed into separate reaction vessels along with a solution containing 0.6 M FFCA in 3:2 (wt/wt) dioxaneiH^O. The powered catalysts were Cu BASF 0602 (reduced in-house), Cu Clariant T-4874, Cu Clariant T-4874* (reduced in-house), Ni JM HTC 500 RP, Pd/C JM-4, Pd/C JM-6, Pd/C JM-10, Pt/C JM-24, Pt/C JM-27, Ru/C JM-37, Ru/C JM-38 and a control without a catalyst. Catalysts Cu BASF 0602* and Cu Clariant T-4874* were used in a further reduced form (350°C in forming gas for 3 hours). Each reaction vessel was pressurized with hydrogen at target pressure of 55 bar. Reaction vessels were heated to a target temperature of 70°C and shaken for 2 hours or, alternatively, reaction vessels were heated to a target temperature of 100°C and shaken for 1 hour. After the reaction was completed, the shaking was stopped and the reactor was cooled down to room temperature.
N-(2,6-dimethoxyphenyl)-5-methylfuran-2-carboxamide[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
59%
With dmap; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; In dichloromethane; at 20℃;
To a solution of 5-methylfuran-2-carboxylic acid (1.0 g, 8.0 mmol, 1 equiv) and 2,6- dimethoxyaniline (1.46 g, 9.5 mmol, 1.2 equiv) in DCM (10 mL) were added DMAP (44 mg, 0.4 mmol, 0.05 equiv) and EDCI (1.5 g, 9.6 mmol, 1.2 equiv) successively at room temperature. The resulting mixture was stirred at room temperature overnight. The reaction mixture was diluted with EtOAc (100 mL), washed with water (3*20 mL) and brine (50 mL), dried over anhydrous Na2S04, and concentrated in vacuo. The residue was purified by flash column chromatography (eluted with PE/EtOAc = 20/1 ~ 1/1) to afford the title compound N-(2,6-dimethoxyphenyl)-5-methylfuran-2-carboxamide as a white solid (1.23 g, 59 % yield). LC-MS: m/z 262.1 (M+H)+
Chemistry
Pharmaceutical Intermediates
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Material Science
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120K+ Compounds
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