Category: 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., SDS of cas: 22227-26-5

Charged 3,5-bis(trifluoromethyl)benzonitrile (100 gm, 1 meq.), 2 (N) Sodium hydroxide (21.7 gm, 1.3 meq.) into 400 ml methanol and stirred the reaction mass at 20 – 30¡ãC for 2-3 hrs. Added Dimethyl sulphoxide (100 ml) followed by dilute 30percent H202 solution (100 gm diluted in 300m1 water, 2.1 eq.) at 20 -35¡ãC. Stirred the mass for 2-3 hrs. at 20-30¡ãC and confirmed reaction completion by HPLC. Reaction mass quenched by addition of water (500 ml, S Vol). Filtered the slurry and washed the wet cake by water (500 ml, SVol). Dried under vacuum at 50-60¡ãC to get 100 gm 3, 5-bis (trifluoromethyl) benzamide (Purity 99 percent). Charged 3, 5-bis (trifluoromethyl) benzamide, prepared according to procedures a or b, as described above, (100 gm, 1 meq) into N, N Dimethyl formamide (100 ml, 1 vol). Added N, N Dimethyl formamide dimethyl acetal (70 gm, 1.5 meq) at 20-30¡ãC and stirred the reaction mass for 2-3 hrs. Reaction completion for the formation N-((dimethylamino)methylene)-3,5- bis(trifluoromethyl)benzamide was confirmed by HPLC. Cooled reaction mass to 10-15¡ãC and added acetic acid (S00 ml, S vol.) followed by hydrazine hydrate (31 gm, 1.5 meq). Reaction mass was heated to S0-SS¡ãC and stirred for 2-3 hrs. at same temparature. Reaction was monitored by HPLC. Cooled reaction mass to 20-30¡ãC and quenched by addition of water (2.S L, 2S vol.). Filtered the slurry and washed the wet cake by water (S00 ml, S vol.). Dried under vacuum at 50-60¡ãC to get 3 -(3,5 -bis(trifluoromethyl)phenyl)- 1 H-i ,2,4-triazole (94 gr, Purity 97percent).

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; WATSON LABORATORIES INC.; MUTHUSAMY, Anantha Rajmohan; KANNIAH, Sundara Lakshmi; RAVI, Akash; DAS, Tonmoy Chitta; CHEMATE, Rajendra Popat; SINGH, Anil Kumar; WAGH, Yogesh Dhananjay; (60 pag.)WO2018/129227; (2018); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 22227-26-5, name is 3,5-Bis(trifluoromethyl)benzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 22227-26-5

General procedure: Benzamide (476 mg, 3.9 mmol) and benzaldehyde(203 mL, 2 mmol) were dissolved in dry DMF (8 mL).TMSCl (507 mL, 4mmol) was added as a catalyst and wasstirred at 50 ¡ãC for 18 h under nitrogen. Awhite precipitatewas formed with the addition of a few drops of water andwas purified by stirring with diethyl ether for 30 min. Theproduct was isolated using vacuum filtration. Yield 31percent

The synthetic route of 22227-26-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Clarke, Harriet J.; Van Rossom, Wim; Horton, Peter N.; Light, Mark E.; Gale, Philip A.; Supramolecular Chemistry; vol. 28; 1-2; (2016); p. 10 – 17;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics