tetraMethyl cyclohexane-1,2,4,5-tetracarboxylate synthesis
- Product Name:tetraMethyl cyclohexane-1,2,4,5-tetracarboxylate
- CAS Number:92298-55-0
- Molecular formula:C14H20O8
- Molecular Weight:316.3
635-10-9
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Yield:-
Reaction Conditions:
with hydrogen in methanol at 180 - 250; under 37503.8 Torr;Reagent/catalyst;Temperature;Pressure;
Steps:
2.2 2) Preparation of hydrogenated pyromellitic acid ethyl ester
Preparation of hydrogenated pyromellitic acid ester: Dissolve tetraethyl pyromellitic acid in anhydrous ethanol.An ethanol solution containing 20% by weight of tetraethyl pyromellitate was formed as a reaction raw material solution.In the inner diameter of 10mm,A SUS316 reaction tube having a length of 100 mm was filled with 5 g of a 1% by weight Ru-1 wt% Pd/Al2O3 catalyst prepared by an impregnation method. In-situ hydrogen was reduced at 250° C., cooled to a temperature of 150° C., and a hydrogen gas pressure of 4 MPa, and a pyromellitic acid ethyl ester 20 wt % ethanol solution was passed at 0.5 mL/min and hydrogen at 30 mL/min for reaction. The conversion of ethyl pyromellitic acid was maintained at approximately 99% from the beginning of the reaction. The selectivity for hydrogenated pyromellitic acid was 98%. The collected reaction solution was decompressed to remove half of the solvent, cooled down to 0 to -10 DEG C, allowed to stand to crystallize, and filtered. The filter cake was washed with cold ethanol and dried at room temperature under reduced pressure to obtain ethyl hydrogenated tetrahydrophthalic acid ethyl ester.
References:
CN108069978,2018,A Location in patent:Paragraph 0036; 0039; 0040; 0064
89-05-4
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