Method for preparing dialkyl 1,4-cyclohexanedicarboxylate
A technology of cyclohexanedicarboxylic acid diester and succinic acid diester, which is applied in the field of preparation of important chemical intermediate 1,4-cyclohexanedicarboxylic acid diester, can solve problems such as increasing equipment cost, and achieve wide development Potential and application prospects
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Embodiment 1
[0021] Embodiment 1: take dimethyl succinate to prepare dimethyl succinate as an example, describe in detail the process of preparing succinate diester by succinate diester: when a thermometer, drop In the 500ml round bottom flask of liquid funnel and fractionating device, add 73g dimethyl succinate, be warming up to reflux under stirring. Under the protection of nitrogen, 20ml of methanol solution of sodium methoxide (containing 5.4g of sodium methoxide) was dropped into the system. After continuing to reflux for 4h, it was cooled. Methanol was added to the system to precipitate a large amount of precipitate, which was filtered by suction and washed with anhydrous methanol to obtain a pale yellow solid. on the obtained solid 1 H NMR and 13 C NMR (eg figure 2 shown).
Embodiment 2
[0022] Example 2: Add 1.0g dimethyl succinylsuccinate, 0.1g reduced Ru / H-β catalyst with a loading capacity of 5wt.%, and 20mL isopropanol into a 50mL autoclave, seal and use The gas in the reactor was replaced by hydrogen 6 times. Then fill it with 10MPa hydrogen, raise the temperature to 120°C with stirring, keep it for 10h, then cool to room temperature, stop stirring, and carefully reduce the pressure to normal pressure. After the catalyst was filtered out, all the products were transferred to a 25mL volumetric flask, and the internal standard mesitylene was added to make up the volume with isopropanol, and then samples were taken to characterize the main products using GC-MS and the gas chromatography retention time of standard substances. The conversion rate of raw material dimethyl succinyl succinate and the selectivity of product dimethyl 1,4-cyclohexanedicarboxylate were obtained by gas chromatographic analysis and quantitative internal standard method. The conversio...
Embodiment 3-12
[0027] These several embodiments have investigated different catalysts, and the reaction conversion rate and product selectivity of 1,4-cyclohexanedicarboxylate prepared by hydrodehydration of diethyl succinylate succinate are affected, specifically as follows :
[0028]Add 1.0g diethyl succinylsuccinate, 0.05g reduced catalyst with a loading capacity of 10wt.%, 0.2g additive, and 20mL isopropanol into a 50mL autoclave, and replace the interior of the autoclave with hydrogen after sealing Gas 6 times. Then fill it with 5MPa hydrogen, raise the temperature to 150°C with stirring, keep it for 6h, then cool to room temperature, stop stirring, and carefully reduce the pressure to normal pressure. After the catalyst was filtered out, all the products were transferred to a 25mL volumetric flask, and the internal standard was added to make up to volume with isopropanol. The product was analyzed according to the method in Example 2, and the conversion rate of diethyl succinosuccinat...
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