Technique for synthesizing ethyl cyanoacetate with interesterification method
A technology of ethyl cyanoacetate and a process method, which is applied in the technical field of synthesizing ethyl cyanoacetate by transesterification, and achieves the effects of simple preparation, overcoming water resistance, and easy storage
Active Publication Date: 2012-03-28
溧阳常大技术转移中心有限公司
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[0006] In summary, hydrotalcite and hydrotalcite-like catalysts have been widely used as heterogeneous catalysts in organic synthesis reactions, especially in esterification and transesterification reactions, but no hydrotalcite or hydrotalcite-like catalysts have been used for methyl cyanoacetate. A report on the synthesis of ethyl cyanoacetate by transesterification with ethanol
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[0013] Example 1. Add 0.6mol ethanol, 0.6mol methyl cyanoacetate and 3.0g hydrotalcite [Mg 0.75 Al 0.25 (OH) 2 (CO 3 ) 0.125 0.5H 2 O], turn on the stirring, gradually warming up to 85°C, and react for 8 hours. The conversion rate of the obtained ethyl cyanoacetate was 58.21%, and the selectivity was 99.18%.
[0014] Example 2. Add 1.2mol ethanol, 0.4mol methyl cyanoacetate and 3.0g hydrotalcite-like [Mg 0.37 Zn 0.24 Al 0.39 (OH) 2 (CO 3 ) 0.20 2.0H 2 O], turn on the stirring, gradually warming up to 80°C, and react for 8 hours. The mixture in the four-necked flask was filtered while hot to recover the catalyst, the recovery rate of the catalyst was 93.12%, the conversion rate of the obtained ethyl cyanoacetate was 78.08%, and the selectivity was 99.48%.
[0015] Example 3. Add 0.6mol ethanol, 0.6mol methyl cyanoacetate and 2.0g hydrotalcite-like [Mg 0.37 Zn 0.24 Al 0.39 (OH) 2 (CO 3 ) 0.20 5.0H 2 O], turn on the stirring, gradually warming up to 85°C, and ...
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The invention relates to a technological method of adopting hydrotalcite or layered double hydroxides as catalysts to catalyze methyl cyanoacetate and ethanol to carry out transesterification to synthesize ethyl cyanoacetate; the manufacturing steps are as follows: (1) adopting the hydrotalcite or the layered double hydroxides as catalysts and a certain amount of the methyl cyanoacetate and the ethanol as reactants, wherein, the molar ratio of the ethanol to the methyl cyanoacetate is 1 to 6 / 1; the used amount of the hydrotalcite or the layered double hydroxides is 1.0 to 6.0 percent of the weight ratio of the total weight of the reactants; (2) opening, stirring and starting to heat to 80 to 85 DEG C with the reaction time of 6 to 12 hours; (3) carrying out immediate filtration and recycling of the catalysts of the reacted mixtures when the mixture is still hot so that the catalysts can be used repeatedly after being dried and activated; (4) carrying out the distillation of the filtered liquid and recycling the incompletely reacted methyl cyanoacetate, the ethanol and the resultant, methanol, to obtain the crude product, ethyl cyanoacetate. The catalysts used in the technological method are characterized by high efficiency, easy preservation, long service life and recoverability.
Description
technical field [0001] The invention relates to a process for synthesizing ethyl cyanoacetate by transesterifying methyl cyanoacetate and ethanol as a catalyst with hydrotalcite or hydrotalcite-like catalyst. Background technique [0002] Ethyl cyanoacetate is an important chemical intermediate, which is widely used in the synthesis of esters, amides, acids, nitriles and other compounds. Ethyl cyanoacetate is processed and condensed under the action of an alkaline catalyst. After dehydration, drying, cracking and distillation under reduced pressure, high-quality instant superglue is obtained. It is mainly used for furniture repair, toy bonding and bonding of other substances. [0003] At present, the domestic and foreign production process of ethyl cyanoacetate mainly includes: ① post-cyanation method, first obtain ethyl chloroacetate by esterification of chloroacetic acid and ethanol, after refining, carry out cyanation reaction with sodium cyanide to obtain cyanoacetate E...
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IPC IPC(8): C07C255/19C07C253/30
CPCY02P20/10
Inventor 邱滔李桂勇
Owner 溧阳常大技术转移中心有限公司