Catalytic synthesis process of methyl succinic acid

A technology of methyl succinic acid and a synthesis method, applied in the field of synthesis of methyl succinic acid, can solve the problems of many operation steps, complicated process and high cost, and achieve the effects of strong catalytic stability, simple operation and simple method

Inactive Publication Date: 2005-04-27
FUDAN UNIV
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  • Abstract
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Problems solved by technology

The process of ester hydrolysis is complicated, with many operation steps, high cost and low yield

Method used

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  • Catalytic synthesis process of methyl succinic acid
  • Catalytic synthesis process of methyl succinic acid
  • Catalytic synthesis process of methyl succinic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0035] Embodiment: 1 is carried out in long 13 centimeters, the intermittent tank reactor of diameter 3.8 centimetres, puts into palladium carbon catalyst (palladium content 5wt%) 1.0g and 10g raw material itaconic acid, adds mixed solvent 10ml ethanol and 50ml THF, After dissolving, check for leaks, pass hydrogen gas, stir, keep constant temperature at 50°C and constant pressure at 2.5atm for hydrogenation reaction. The reaction was basically completed after 12 hours. Sedimentation, filtration, vacuum distillation, drying. The obtained product has a conversion rate of 99.15% and a selectivity of 99.95%.

[0036] Embodiment: 2 same reaction apparatus, with 18g palladium-carbon catalyst (w0.25%) 10g raw material, mixed solvent ratio is 0ml ethanol / 60ml tetrahydrofuran, 10 ℃, 1.0atm, reacted 16 hours, obtained product transformation rate 99.83%, The selectivity is 99.67%.

[0037] Embodiment: 3 same as above reaction apparatus, with 0.15g (w10%) catalyst 10g raw material, mix...

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PUM

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Abstract

The present invention is catalytic synthesis process of methyl succinic acid. The present invention adopts Pd/C catalyst and itaconic acid as material to synthesize methyl succinic acid through liquid phase hydrogenation in certain mixed solvent. The reaction is completed at 10-80 deg.c; and the coarse product is purified through re-crystallization inside cold ethyl ether to reach methyl succinic acid content over 99 %. The said preparation process has mild reaction condition, short reaction time, high itaconic acid conversion rate of 98-99 % and high selectivity of 99 %.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to a synthesis method of methylsuccinic acid. Background technique [0002] The molecular formula of methylsuccinic acid is C 5 h 8 o 4 , the English name is methylsuccnic acid, a chiral compound (CA registration number is [498-21-5], (+-)[630-60-2], R[3641-51-8], S[2174-58 -5]), white prismatic crystals, widely used, generally used, waste paper bleaching, etchant, esterification reaction, photochemical reaction, chiral molecules have a wide range of uses, and are used to synthesize a large number of chiral compounds and pharmaceutical macromolecules indispensable reagents. [0003] There are many methods for synthesizing methylsuccinic acid in the existing literature, which can be roughly divided into two categories: chiral synthesis and achiral synthesis. [0004] There are two routes for chiral synthesis. One is that Mateoli, Tefort, Dawson et al. use itacon...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/36C07C55/02
Inventor 史焕聪沈伟徐华龙
Owner FUDAN UNIV
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