40134-18-7Relevant articles and documents
Preparation method of 2-chloro-N, N-dimethyl nicotinamide
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Paragraph 0010; 0025-0026; 0028-0029; 0031-0032, (2021/03/13)
The invention belongs to the technical field of pesticides, and particularly relates to a preparation method of 2-chloro-N, N-dimethyl nicotinamide. The preparation method of the 2-chloro-N, N-dimethyl nicotinamide comprises the following steps of taking 2-chloronicotinic acid as a raw material, and carrying out esterification reaction with methanol to obtain 2-chloronicotinic acid methyl ester, and carrying out aminolysis reaction with dimethylamine in the presence of a catalyst N, N-dimethyl nicotinamide to obtain the 2-chloro-N, N-dimethyl nicotinamide. The preparation method disclosed by the invention is mild and controllable in reaction, simple in process equipment, low in dimethylamine consumption, low in production cost and good in product quality, and the amount of wastewater is greatly reduced and is easy to treat.
A ultrasonic process for synthesizing 2 - halogenated nicotinate and intermediates thereof
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Paragraph 0057; 0058; 0061, (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.
Towards new sila- Or germa-derivatives of motesanib
Boddaert, Thomas,Querolle, Olivier,Meerpoel, Lieven,Angibaud, Patrick,Maddaluno, Jacques,Durandetti, Muriel
, p. 1210 - 1218 (2019/07/31)
– Developing new access to original silylated heterocycles is an emerging challenge in medicinal chemistry. In this paper, we describe a synthesis of silylated and germylated Motesanib analogues relying on a peptide coupling between a nicotinic acid derivative and silylated or germylated heterocycles, prepared according to our previous reports.