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ChemicalBook CAS DataBase List ITACONIC ACID MONO-N-BUTYL ESTER
6439-57-2

ITACONIC ACID MONO-N-BUTYL ESTER synthesis

5synthesis methods
-

Yield:-

Reaction Conditions:

with hierarchical mesoporous zeolites at 100; for 6 h;Overall yield = 95.2 %; chemoselective reaction;Reagent/catalyst;Time;

Steps:

2.4 Catalytic reactions
Before esterification, all the catalysts were ion exchanged with 1 M NH4NO3 for three times and calcined to convert the zeolites into H+ form. In a typical reaction, 0.1 mol itaconic acid (13 g) and 0.3 mol n-butyl alcohol (22.23 g) with 2 g decane as internal standard were added into the three-neck flask equipped with a reflux condenser. When the temperature was stabilized at 100 °C, 0.26 g catalysts after drying at 150 °C for 2 h to eliminate adsorbed water were added into the reacting system. The samples were periodically taken and analyzed by GC-MS (Agilent, 6890/5973 N). The yields of monobutyl itaconate and dibutyl itaconate were given by drawing a standard curve by using decane as internal standard to determine the concentration of corresponding substances. In recycling tests, hierarchical porous zeolites (HMZ and HNZ) and traditional ZSM-5 zeolites were separated from reaction system, dried at 100 °C for 2 h, and then added to fresh substrate solution. The reaction time duration was limited to 6 h according to the catalytic activity shown in the first catalytic experiment. After three recycles, catalysts were calcined at 550 °C for 6 h to eliminate the coke deposition and then reused to investigate the catalytic activity.

References:

Zhu, Yan;Hua, Zile;Song, Yudian;Wu, Wei;Zhou, Xiaoxia;Zhou, Jian;Shi, Jianlin [Journal of Catalysis,2013,vol. 299,p. 20 - 29]

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