22227-26-5, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 22227-26-5, name is 3,5-Bis(trifluoromethyl)benzamide, A new synthetic method of this compound is introduced below.
A, 1560 g of intermediate 2,6.24 L of ~ N ‘N-dimethylformamide was charged into a 50 L autoclave, and the reaction was cooled to 12 ¡ã C; B, adding sodium hydroxide in batches, And control the reaction system temperature does not exceed 15 ¡ã C, Add to continue stirring 20min; C, the reaction system is cooled to 10 ¡ã C, adding the magnesium chloride hexahydrate to the reaction system, the temperature of the reaction system is 10 ~ 15 D, the reaction system to room temperature, stirring 4h; E, with hydrochloric acid to adjust the reaction system pH to 2.2, and the body reaction system temperature below 20 ¡ã C; F was added to the reaction system by the addition of 5 L of methyl tert-butyl ether, and the layers were separated and then extracted with methyl tert-butyl ether (2.5 L X). The organic layers were combined and washed with saturated sodium chloride (2.5 LX 2); G, concentrated, the residue was added to petroleum ether beating and dried at room temperature to give 1931 g of intermediate 5;H, 1.9 kg of intermediate 5 and 8.9 kg of methanol were charged into a 50 L autoclave, and the reaction was cooled to 10 ¡ã C; I, dropping formylhydrazide into the reaction system; J, the reaction system to cool to 0 ¡ã C; K, 666 g of ethyl formate was added dropwise and the temperature was controlled at 0 to 5 ¡ã C; L, the reaction system temperature to 90 ~ 95 ¡ã C, and at this temperature for 6h; M, the reaction system to cool to 35 ~ 40 ¡ã C, and then to the reaction system by adding 28L of water; N, the addition of methyl tert-butyl ether 12L extraction, standing after the separation, the water phase and then 10L methyl tert-butyl ether extraction; combined organic layer, with saturated sodium chloride (6L X 2) O, the solvent was removed, the crude product was beaten with methylene chloride 3L at room temperature, filtered and dried to give 1.28 kg of intermediate 4 with a liquid phase purity of 98.6percent.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Guangzhou Wenhao Biological Technology Co., Ltd.; Chen Xinying; Xu Liang; Liu Wenzhong; (6 pag.)CN106831617; (2017); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics