53087-78-8Relevant articles and documents
A ultrasonic process for synthesizing 2 - halogenated nicotinate and intermediates thereof
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Paragraph 0047; 0048, (2018/04/21)
The invention discloses a method for synthesizing 2-halogenated ester nicotinate and a 2-halogenated ester nicotinate intermediate according to an ultrasonic method. The method comprises the following steps: adding substituent amino acrolein, a catalyst and cyanacetic ester into a reactor for a reaction under ultrasonic radiation; tracing the reaction till substituent amino acrolein is disappeared, thereby obtaining a reaction solution I containing the 2-halogenated ester nicotinate intermediate; then, adding halogen hydride into the reaction solution I for another reaction to obtain a reaction solution II; tracing and monitoring the reaction till completion; adding a lye into the reaction solution II to adjust the pH value of the reaction solution II to be 5-6; carrying out standing stratification to obtain a water layer and an organic layer; conducting extraction on the water layer by utilizing an organic solvent, and then combining the extraction solution with the organic layer; carrying out refining to obtain 2-halogenated ester nicotinate. Through the adoption of the method, an organic synthesis reaction can be effectively facilitated, the reaction speed and yield can be improved, and the environmental protection can be promoted; the reaction time is short and the operation is simple, that is, the organic synthesis reaction can be finished within 2 hours in general; the product yield and quality are high; specifically, the product yield can reach 90% or higher, and exceed that achieved according to the conventional solvent heating reflux method.
An ionic liquid method of synthesizing 2 - halogenated nicotinate and intermediates thereof
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Paragraph 0049; 0050; 0051; 0052, (2017/10/13)
The invention discloses a method for synthesizing 2-halogenated nicotinate and an intermediate thereof through an ionic liquid method. The method comprises the steps that cyan-acetic ester, ionic liquid and substituted amino acrolein are evenly mixed and heated to a preset temperature for conducting a reaction, the reaction is tracked till the substituted amino acrolein disappears, reaction liquid is cooled to the room temperature and extracted for multiple times through organic solvents, the residual phase of the ionic liquid is reused after being washed and dried, and the intermediate of the 2-halogenated nicotinate is obtained by evaporating the organic solvents from the organic phase; when the 2-halogenated nicotinate is synthesized, the organic solvents do not need to be separated from the intermediate of the 2-halogenated nicotinate, the reaction is continuously conducted by adding hydrogen halide into the organic phase, and the tracking monitoring is conducted till the reaction is completed; the 2-halogenated nicotinate product is prepared after separation. The synthesizing method of the 2-halogenated nicotinate has the advantages of being green and environmentally friendly, easy to operate, high in product yield and good in quality of the synthesized product.
