Category: 123-32-0

Electric Literature of 123-32-0, These common heterocyclic compound, 123-32-0, name is 2,5-Dimethylpyrazine, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Preparation of 3,6-dimethyl-2- (4-trifluoromethyl) benzoyl pyrazine, comprising the steps of:(1) 2,5-dimethyl pyrazine take 0.2mmol, 3- trifluoromethylbenzoyl acid 0.4mmol, silver phosphate 0.02mmol, potassium persulfate 0.4mmol, 1.4mL was added dichloromethane, 0.6mL after the mixture was prepared with distilled water, and the mixture was placed in a reaction tube of 5mL was heated in an oil bath at 40 , the reaction 24h, cooled to room temperature to obtain a reaction solution;(2) The step (1) the resulting reaction mixture was directly concentrated to give a concentrate, the concentrate with ethyl acetate / petroleum ether = 1/2 (v / v) as the developing solvent, separation by thin layer chromatography to give 45mg target The product, in 43% yield.

The synthetic route of 123-32-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Henan Agricultural University; Wu Zhiyong; Zhao Mingqin; Li Yuan; (10 pag.)CN108101856; (2018); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

Electric Literature of 123-32-0,Some common heterocyclic compound, 123-32-0, name is 2,5-Dimethylpyrazine, molecular formula is C6H8N2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: A 25 mL Schlenk tube equipped with a magneticstirring bar was charged with2,6-lutidine (0.75 mmol, 3equiv.), p-nitro-benzaldehyde(0.25 mmol), dioxane/water(1:1, 1ml) and [Hmim][H2PO4](1equiv.).The tube was sealed and heated at 100 for 24h. Aftercompletion of the reaction, the resulting solution was extracted with ether (3¡Á10 ml). The organic layer was dried with anhydrous Na2SO4,and concentrated under vacuum. The residue was chromatographed on a silica gelcolumn eluted with a mixture of petroleum ether and ethyl acetate (1:1) to givepure products (92%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,5-Dimethylpyrazine, its application will become more common.

Reference:
Article; Zhang, Xue-Yan; Dong, Dao-Qing; Yue, Tao; Hao, Shuang-Hong; Wang, Zu-Li; Tetrahedron Letters; vol. 55; 40; (2014); p. 5462 – 5464;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

123-32-0, Name is 2,5-Dimethylpyrazine, 123-32-0, belongs to Pyrazines compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows.

To the ethyl acetate solution (7 ml) of 2,5-dimethylpyrazine (500 mg, 5.36 mmol) at room temperature, m-chloroperbenzoic acid (1.27 g, 7.36 mmol) was added and stirred for 24 hours did. Thereafter, the reaction system was filtered and the solid was washed with ethyl acetate to obtain 2,5-dimethylpyrazine-N, N’-dioxide. Yield 517 mg, yield 80%, white solid

Statistics shows that 2,5-Dimethylpyrazine is playing an increasingly important role. we look forward to future research findings about 123-32-0.

Reference:
Patent; NIPPON STEEL & SUMIKIN CHEMICAL COMPANY LIMITED; KYUSHU INSTITUTE OF TECHNOLOGY; NAGAHAMA, TAKUO; KAWADA, ATSUSHI; TAKASHIMA, WATARU; OKAUCHI, TATSUO; NAGAMATSU, SHUICHI; (69 pag.)JP2017/178911; (2017); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

123-32-0, 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. 123-32-0, name is 2,5-Dimethylpyrazine, A new synthetic method of this compound is introduced below.

In a 500-L reactor equipped with a reflux condenser, 250 kg of water and 20 kg of 2,5-dimethylpyrazine were added.Potassium permanganate 4.0kg, heated to 82C, kept at 80C for 1.6h, the solution purple faded and cooled to 76C,Then add 4.0kg of potassium permanganate, slowly warming to 82C, and hold at 82C for 1.6h.The solution purple faded and then incubated for 2.5 hours, and the temperature was reduced to 22 DEG C.; the filter cake was filtered, the filter cake was washed with 12 kg of water, and the filtrate was combined;The combined filtrate is first concentrated under normal pressure, distilled out of water and pyrazine solution (recovery application), after about 82% steaming,Diverted under reduced pressure to dryness; which distilled out of the filtrate 250kg, containing 2,5-dimethyl pyrazine 17kg;Add 15kg of water to the steamed kettle and raise the temperature to 52C to fully dissolve it; then pump it to a neutralization kettle., Adjust the pH to 2.5 with 1+1 sulfuric acid at about 6Kg, and extract with butanone (80Kg x 3) 3 times at 52 C to combine the organic phases;The organic phase was allowed to stand for 24 hours and a small amount of water was removed in the lower layer. The upper organic layer was degassed to dryness at atmospheric pressure.Add 10kg of water to heat and dissolve it, and while it is hot, the filtrate is cooled to 0C, crystallized, and suction filtered.The crude product was dried to 3.6kg; recrystallized from butanone to give 3.2kg of light yellow crystalline powder of 5-methylpyrazine-3-carboxylic acid.The yield was 81.6% and the purity was 99.4%.

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; Changzhou Engineering Polytechnic College; Chen Huiru; Chen Wenhua; Huang Yibo; Zhang Yuxiu; (7 pag.)CN108017586; (2018); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

These common heterocyclic compound, 123-32-0, name is 2,5-Dimethylpyrazine, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. 123-32-0

The method of preparing 3,6-dimethyl-2- (4-fluoro) benzoyl pyrazine, comprising the steps of:(1) 2,5-dimethyl pyrazine take 0.2mmol, 4- fluoro-benzoyl acid 0.4mmol, silver phosphate 0.02mmol, potassium persulfate 0.4mmol, 1.4mL was added dichloromethane, 0.6mL distilled water was added, and the mixture was placed in a reaction tube in 5mL, 40 oil bath was heated, reaction 24h, cooled to room temperature to obtain a reaction solution;(2) The step (1) the resulting reaction mixture was directly concentrated to give a concentrate, the concentrate with ethyl acetate / petroleum ether = 1/2 (v / v) as the developing solvent, separation by thin layer chromatography to give 34 mg desired product in 74% yield.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 123-32-0.

Reference:
Patent; Henan Agricultural University; Wu Zhiyong; Zhao Mingqin; Li Yuan; (10 pag.)CN108101856; (2018); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 123-32-0 name is 2,5-Dimethylpyrazine, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 123-32-0

Intermediate 55 2-(chloromethyl)-5-methylpyrazine To a solution of 2,5-dimethylpyrazine (500 mg, 4.62 mmol) in carbon tetrachloride (7 mL) was added NCS (679 mg, 5.09 mmol) followed by BPO (20 mg) and the mixture was heated to 80 C for 6 hours. The mixture was diluted with DCM and extracted with saturated aqueous sodium sulfite solution and brine. The organic layer was dried and concentrated to give a crude product which was purified via silica gel chromatography eluting with petroleum ether/ ethyl acetate (1 :0 to 15: 1) to give 2-(chloromethyl)-5-methylpyrazine (133 mg, 20.19% yield) as yellow oil. LCMS retention time 0.557 min; LCMS MH+ 143.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,5-Dimethylpyrazine, and friends who are interested can also refer to it.

Reference:
Patent; HYDRA BIOSCIENCES, INC.; CHENARD, Bertrand; GALLASCHUN, Randall; WO2014/143799; (2014); A2;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

Some common heterocyclic compound, 123-32-0, name is 2,5-Dimethylpyrazine, molecular formula is C6H8N2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. 123-32-0

(b) 3,6-Dimethylpyrazin-2-amine A mixture of 2,5-dimethylpyrazine (14 g, 0.13 mol) in N,N-dimethylaniline (50 mL) was heated to 170 C. and NaNH2 (22 g, 0.56 mol) was added in portions. The reaction mixture was stirred at 170 C. for 1 h, and the solvent was removed. The product was purified by silica gel column chromatography to give 3,6-dimethylpyrazin-2-amine as a brown solid (1.6 g, yield 10%). ESI MS: m/z 124 [M+1]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 123-32-0, its application will become more common.

Reference:
Patent; Sunovion Pharmaceuticals Inc.; US2012/178748; (2012); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

123-32-0, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 123-32-0 as follows.

A method for preparing 5-methylpyrazine-2-carboxylic acid by catalytic oxidation, firstly, diatomaceous earth, manganese chloride, sodium tungstate,Cobalt nitrate and distilled water were added to the reactor at the following element mass ratio: diatomaceous earth: Mn:W:Co:H2O=1:0.09:0.08:0.14:50,Magnetically stirring at room temperature to make it dispersed and uniformly adsorbed, and then removing water by evaporation.Adding a liquid silica sol with a total mass of 5% of the solid sample and kneading it into a small granular sample of 1-2 mm.The mixture was placed in a muffle furnace and calcined in an air atmosphere at 600 C for 5 hours to obtain Mn-W-Co/diatomaceous earth-supported catalyst particles.10 g of Mn-W-Co/diatomaceous earth catalyst particles were packed into a fixed bed microreactor reaction tube, and the reactor was heated to 330 C.The reaction raw material 2,5-dimethylpyrazine was introduced into a fixed bed reaction tube by bubbling with high-temperature steam at 10 ml/min.Oxygen is introduced into the reaction tube separately at 20 ml/min to cause catalytic oxidation of 2,5-dimethylpyrazine in the catalytic bed.The 5-methylpyrazine-2-carboxylic acid is produced and taken out of the reaction tube by water vapor, condensed, crystallized, and collected.Analysis of 5-methylpyrazine-2-carboxylic acid by gas chromatographyThe yield was 75.6%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 123-32-0, and friends who are interested can also refer to it.

Reference:
Patent; Lanzhou University; Dong Zhengping; (6 pag.)CN109369544; (2019); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

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. 123-32-0, name is 2,5-Dimethylpyrazine, A new synthetic method of this compound is introduced below., 123-32-0

Preparation of 3,6-dimethyl-2- (3-methoxy) benzoyl pyrazine, comprising the steps of:(1) 2,5-dimethyl pyrazine take 0.2mmol, 3- methoxybenzoyl acid 0.4mmol, silver phosphate 0.02mmol, potassium persulfate 0.4mmol, 1.4mL was added dichloromethane, 0.6mL of distilled water was added, and the reaction mixture was placed in a 5mL tube and placed in an oil bath at 40 heated, reaction 24h, cooled to room temperature to obtain a reaction solution;(2) The step (1) the resulting reaction mixture was directly concentrated to give a concentrate, the concentrate with ethyl acetate / petroleum ether = 1/2 (v / v) as the developing solvent, separation by thin layer chromatography to give 32mg target The product, in 66% yield.

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; Henan Agricultural University; Wu Zhiyong; Zhao Mingqin; Li Yuan; (10 pag.)CN108101856; (2018); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

123-32-0, These common heterocyclic compound, 123-32-0, name is 2,5-Dimethylpyrazine, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Preparation of 3,6-dimethyl-2- (4-methylphenyl) benzoyl pyrazine, comprising the steps of: (1) Take 0.2 mmol 2,5-dimethyl pyrazine, methyl benzoyl formate 0.4mmol, 0.02 mmol silver phosphate, potassium persulfate 0.4mmol 5mL reaction tube was placed in dichloromethane was added 1.4mL , 0.6 mL of distilled water was added, and the mixture was placed in an oil bath at 40 heated, reaction 24h, cooled to room temperature to obtain a reaction solution;(2) The step (1) the resulting reaction mixture was directly concentrated to give a concentrate, the concentrate with ethyl acetate / petroleum ether = 1/2 (v / v) as the developing solvent, separation by thin layer chromatography to give 39mg target The product yield was 87%.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 123-32-0.

Reference:
Patent; Henan Agricultural University; Wu Zhiyong; Zhao Mingqin; Li Yuan; (10 pag.)CN108101856; (2018); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem