Category: 41270-66-0

Electric Literature of 41270-66-0, The chemical industry reduces the impact on the environment during synthesis 41270-66-0, name is 5-Chloro-2,3-diphenylpyrazine, I believe this compound will play a more active role in future production and life.

A 2-butanone / water mixed solution (360 mL of 2-butanone and 22 mL of water) was placed,To the mixture was added sodium iodide 28g,Stir well after adding a starting material 22g, heated to reflux, smooth, add HI solution 8mL,Reflux overnight (due to the difference between raw material and product polarity, TLC can not track monitoring)The liquid phase was monitored to about 5% of the raw material (the reaction liquid was no longer reduced after 1 hour). The reaction mixture was filtered, the residue was washed with 4 mL of 2-butanone, the combined filtrates were swirled to remove the solvent,NaHSO3 0.7g aqueous solution 40mL, stir, then the solution was acidic, with stirring NaOH solid was added until the solution was strong alkaline, stirring to alkaline no longer change, filtration, the filter cake was recrystallized from methanol to give Compound 1 Dark yellow solid 17.8g,Yield 60.1%, purity 97.74%.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 5-Chloro-2,3-diphenylpyrazine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nanjing Aide Kaiteng Bio-pharmaceutical Co., Ltd.; Wang Xuegen; He Lingyun; Wei Chao; Yu Yang; (6 pag.)CN106957269; (2017); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 41270-66-0, name is 5-Chloro-2,3-diphenylpyrazine, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C16H11ClN2

To a solution of 1.00 g of 2-chloro-5,6-diphenylpyrazine in 10 ml of methanol, 2.14 g of allylamine was added and the mixture was reacted in a sealed tube at 80C for 41 hours, followed by stirring at room temperature for 54 hours.. After the solvent was evaporated under reduced pressure, the reaction solution was combined with water, extracted with chloroform, dried over anhydrous magnesium sulfate, and then the solvent was evaporated under reduced pressure.. The residue was purified by silica gel column chromatography to obtain 330 mg of the desired compound as a pale yellow crystal having a melting point of 97 to 100C

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 41270-66-0.

Reference:
Patent; Nippon Shinyaku Co., Ltd.; EP1400518; (2004); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

Synthetic Route of 41270-66-0, These common heterocyclic compound, 41270-66-0, name is 5-Chloro-2,3-diphenylpyrazine, 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.

In a 10 liter reactor, 2 liters of isopropylamine and 222 g of SLP-3 were added and the reaction was stirred at room temperature for 48 hours until the reaction was completed.Add 5 liters of ethyl acetate and 3 liters of water to stir, and let stand for phase separation; the organic phase is washed with dilute hydrochloric acid, water and saturated sodium bicarbonate, dried over anhydrous sodium sulfate, filtered and concentrated to obtain crude product; crude product is ethyl acetate. Recrystallization from petroleum ether gave 205 g of white solid SLP-4.Yield: 85%.1H NMR (400 MHz, CDCl3): delta 7.89 (s, 1H), 7.43-7.22 (m, 10H), 4.59 (d, 1H), 4.08 (m, 1H), 1.30 (d, 6H)ESI/MS+(m/z):289

The synthetic route of 41270-66-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Aikangrui Pharmaceutical Technology Co., Ltd.; Fan Linfeng; Zhu Yangwei; Qiu Aiyun; Lv Bojie; Xu Zhonghui; Zhang Changxuan; (11 pag.)CN106316967; (2017); A;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

Adding a certain compound to certain chemical reactions, such as: 41270-66-0, name is 5-Chloro-2,3-diphenylpyrazine, belongs to pyrazines compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 41270-66-0, Computed Properties of C16H11ClN2

5-Chloro-2,3-diphenylpyrazine (300 gm), 4-isopropylaminobutanol (443 gm) were taken and then heated to 170 – 195 C, stirred for 10 hours to 12 hours and further cooled to 25- 30C. Then added water, extracted with methyl tert-butyl ether, dried the organic layer and concentrated to obtain the desired compound. Yield: 252 gm Chromatographic Purity (by HPLC): 99.01%

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; HONOUR (R&D); PARTHASARADHI REDDY, Bandi; RATHNAKAR REDDY, Kura; SUBHASH CHANDER REDDY, Kesireddy; VAMSI KRISHNA, Bandi; RAJENDAR REDDY, Kancharla; (25 pag.)WO2017/168401; (2017); A1;,
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. 41270-66-0, name is 5-Chloro-2,3-diphenylpyrazine, A new synthetic method of this compound is introduced below., Formula: C16H11ClN2

To a solution of 1.58 g of 2-chloro-5,6-diphenylpyrazine in 10 ml of triethylamine, 1.20 g of 5-(2-tetrahydropyranyloxy)-1-pentyne, 208 mg of dichlorobis(triphenylphosphine) palladium (II) and 56 mg of copper (I) iodide were added, followed by stirring under an argon atmosphere at 80C for 8 hours.. The solvent was evaporated under reduced pressure and the residue was dissolved in diethyl ether, and then the insoluble matter was removed by filtration through celite.. After the solvent was evaporated under reduced pressure, the residue was purified by silica gel column chromatography to obtain 1.79 g of the desired compound as a brown oily substance.

The synthetic route of 41270-66-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nippon Shinyaku Co., Ltd.; EP1400518; (2004); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

Synthetic Route of 41270-66-0, 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. 41270-66-0 name is 5-Chloro-2,3-diphenylpyrazine, 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] Step 1. 2-(1.1.2.2.3.3.4.4-dg-4-((5.6-Diphenylpyrazin-2-yl)(propan-2-yl)amino)butan- l-ol (12b). To a solution of commercially available 5-chloro-2,3-diphenylpyrazine (10) (0.57 g, 2.14 mmol) in NMP (2.0 mL), was added d7-aminoalcohol lib (0.75 g, 5.35 mmol, 2.5 equiv, prepared as described in Example 10). The reaction vessel was sealed and heated to 190 0C for 15 hours, then cooled to ambient temperature. The mixture was diluted with ice water and extracted with Et2O (3 x 20 mL). The combined organic layers were washed successively with water and brine. The resulting organic layer was dried (MgSO4), filtered and concentrated in vacuo. The resulting residue was purified by column chromatography (SiO2, 30-50% EtO Ac/heptane) to afford 12b (0.20 g, 25%). MS (M+H): 370.0

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Chloro-2,3-diphenylpyrazine, and friends who are interested can also refer to it.

Reference:
Patent; CONCERT PHARMACEUTICALS, INC.; HARBESON, Scott L.; MASSE, Craig E.; LIU, Julie F.; WO2011/17612; (2011); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

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 41270-66-0 as follows. Computed Properties of C16H11ClN2

In one embodiment of the preparation method of the sirepag intermediate of the present invention, the preparation method of the siriparg intermediate according to the present embodiment is: in a reaction bottle equipped with a reflux tube, a drying tube and a thermometer, adding 5- Chloro-2,3-diphenylpyrazine (30.0 g, 0.11 mol, 1.0 eq.), 4-(isopropylamino)-1-butanol (18.5 g, 0.14 mol, 1.25 eq.), 1, 4-Dioxane 150 mL, stir and dissolve, and then add Pd (dba)2(2.4g, 4.2mmol), P(o-tolyl)3(1.69 g, 8.3 mmol), sodium tert-butoxide (13.0 g, 0.135 mol), heated to 120 C., and incubated for 1.8 hours. The reaction was complete by TLC and the reaction was stopped.The mixture was cooled to room temperature and filtered. The filtrate was adjusted to pH 6.5-7.5 with 1N hydrochloric acid, extracted with ethyl acetate (150 mL x 2), washed with 150 mL of brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure with the residue being ethanol: The mixture was recrystallized with 300 mL of n-hexane = 1:15 mixed solvent and dried in an oven to obtain 39.0 g of a white solid. The yield was 96%, and the liquid purity was 97.1%.

According to the analysis of related databases, 41270-66-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Guangdong Saifeng Pharmaceutical Technology Co., Ltd.; Feng Wenzhou; Chen Rongmin; Ding Xiaoming; Zheng Yuchun; Bao Changxiao; Gong Zihua; (9 pag.)CN107652243; (2018); 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. 41270-66-0, name is 5-Chloro-2,3-diphenylpyrazine, A new synthetic method of this compound is introduced below., HPLC of Formula: C16H11ClN2

[131] Step 1. 2-(4-((5,6-Diphenylpyrazin-2-yl)(perdeutero-propan-2-yl)amino)butan-l-ol(12c). To a solution of commercially available 5-chloro-2,3-diphenylpyrazine (10) (0.70 g, 2.62 mmol) in NMP (2 mL), was added d7-aminoalcohol lie (0.54 g, 3.93 mmol, 1.5 equiv, prepared as described in Example 7). The reaction vessel was sealed and heated to 190 0C for 15 hours, then cooled to ambient temperature. The mixture was diluted with ice water and extracted with Et2O (3 x 20 rnL). The combined organic layers were washed successively with water and brine. The resulting organic layer was dried (MgSO4), filtered and concentrated in vacuo. The resulting residue was purified by column chromatography (SiO2, 30-50% EtOAc/heptane) to afford 12c (0.20 g, 21%). MS (M+H): 369.2.

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.

Some common heterocyclic compound, 41270-66-0, name is 5-Chloro-2,3-diphenylpyrazine, molecular formula is C16H11ClN2, 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. Quality Control of 5-Chloro-2,3-diphenylpyrazine

116] Step 1. 2-(1.1.2.2.3.3.4.4-dR-4-((5.6-Diphenylpyrazin-2-viyperdeutero-propan-2- yl)amino)butan-l-ol (12a). To a solution of commercially available 5-chloro-2,3- diphenylpyrazine (10) (0.56 g, 2.10 mmol) in NMP (2.1 mL) was added dis-aminoalcohol 11a (0.46 g, 3.15 mmol, 1.5 equiv, prepared as described in Example 8). The reaction vessel was sealed and heated to 190 0C for 15 hours, then cooled to ambient temperature. The mixture was diluted with ice water and extracted with Et2O (3 x 20 mL). The combined organic layers were washed successively with water and brine. The resulting organic layer was dried (MgSO4), filtered and concentrated in vacuo. The resulting residue was purified by column chromatography (SiO2, 30-50% EtO Ac/heptane) to afford 12a (0.13 g, 16%). MS (M+H): 377.0.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 41270-66-0, its application will become more common.

Reference:
Patent; CONCERT PHARMACEUTICALS, INC.; HARBESON, Scott L.; MASSE, Craig E.; LIU, Julie F.; WO2011/17612; (2011); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem

Reference of 41270-66-0, A common heterocyclic compound, 41270-66-0, name is 5-Chloro-2,3-diphenylpyrazine, molecular formula is C16H11ClN2, 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.

30 g of 2-chloro-5,6-diphenylpyrazin and 131.22 g (0.3 mol) of 4-isopropylamino-1-butanol were added into a 500 mL flask, the mixture was heated to 190 C. and reacted at this temperature for 10 hours, cooled, samples were taken for testing, HPLC purity of the product was 63.5%. The reaction solution was poured into 1 L of ice water, the mixture was extracted with ether 200 mL¡Á3, the organic phases were combined and the solvent was concentrated to dryness, then the residue was purified by column chromatography, and 22.96 g of 4-[N-(5,6-diphenylpyrazin-2-yl)-N-isopropylamino]-1-butanol was obtained, HPLC purity was 97.2%, the molar yield was 56%. (0083) 1H-NMR data: 1H-NMR (400 MHz, CDCl3) delta 8.02 (s, 1H), 7.46 (d, 2H, J=7.6 Hz), 7.36 (d, 2H, J=7.2 Hz), 7.28-7.22 (m, 6H), 4.80-4.78 (m, 1H), 3.71 (t, 2H, J=6.4 Hz), 3.45 (t, 2H, J=7.6 Hz), 1.77-1.74 (m, 2H), 1.66-1.64 (m, 2H), 1.29 (d, 6H, J=6.8 Hz).

The synthetic route of 41270-66-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Seasons Biotechnology (Taizhou) Co., Ltd.; TANG, Fanghui; MA, Chi; JIA, Qiang; (11 pag.)US2018/29998; (2018); A1;,
Pyrazine – Wikipedia,
Pyrazine | C4H4N2 – PubChem