113898-56-9Relevant articles and documents
A ultrasonic process for synthesizing 2 - halogenated nicotinate and intermediates thereof
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Paragraph 0054; 0055, (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.
Method using hydrothermal method to synthesize 2-halogeneated nicotinate and 2-halogeneated nicotinic acid
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, (2017/11/01)
The invention discloses a method using a hydrothermal method to synthesize 2-halogeneated nicotinate and 2-halogeneated nicotinic acid and relates to the field of chemical synthesizing. The method uses substituted amino acrolein, catalyst, catalyst assistant, water and cyanoacetate as raw materials to synthesize the 2-halogeneated nicotinate and the 2-halogeneated nicotinic acid through the hydrothermal method. Compared with the prior art, the method is environmentally friendly, easy in separation, high in product yield, good in product quality, capable of achieving large-scale industrial production favorably, and the like.
Preparation of 2-Fluoropyridines via Base-Induced Decomposition of N-Fluoropyridinium Salts
Umemoto, Teruo,Tomizawa, Ginjiro
, p. 1726 - 1731 (2007/10/02)
N-Fluoropyridinium salts with either BF4-, SbF6-, or PF6- as a counteranion were treated with excess base such as triethylamine at room temperature to give 2-fluoropyridine in good yield.This method was succesfully applied to the preparation of 2-fluoropyridine derivatives possessing electron-donating or -withdrawing substituents using substituted N-fluoropyridinium tetrafluoroborates.Pyridine-F2 compounds produced through reactions of pyridines with molecular fluorine were also treated with base to give 2-fluoropyridines but in low yields.These reactions are considered to occur through a carbene mechanism as follows: a novel N-F-containing cyclic carbene (3), generated from the N-fluoropyridinium salts by 2-proton abstraction, reacts with fluorine atoms from counteranions such as BF4-, SbF6-, or PF6-, followed by elimination of F- from the N-F moiety, to yield 2-fluoropyridines.Previously reported findings in reactions of pyridines with molecular fluorine are explained on the basis of this mechanism.
