Category: 1003-68-5

Electric Literature of 1003-68-5, 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. 1003-68-5, name is 5-Methylpyridin-2(1H)-one, molecular formula is C6H7NO, The 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.

5-methyl-2-pyridone (2) (20 g, 0,18 mol), K2C03 (30,4 g, 0,22 mol), NaOAc (3 g, 0,036 mol, 0,2 mol eq), CuBr (2,62 g, 0,018 mol, 0.1 mol eq) [or Cu20 (1 ,29 g, 0,05 mol eq)], Bromobenzene (4) (40,28 g, 0,26 mol, 1 ,4 mol eq) and DMSO (10 mL, 0,5 V eq) was placed in a round bottom flask under a nitrogen atmosphere. Flask was heated to 135-140C and stirred at this temperature for 6-8 h. After the completion of the reaction according to HPLC analysis, reaction medium was cooled down to about 60 C. Then, 100 mL water was added to the reaction mixture followed by 4 mL NH4OH and 100 mL toluene. The resulting mixture was stirred for 15 min and the phases were separated. Aqueous phase was extracted with 2×50 mL toluene then organic phases were combined (all extractions were carried out at about 60C). Combined organic phases were filtered over a bed of celite after treatment with charcoal. After evaporation of toluene to the dryness, 36,3 g crude pirfenidone was obtained. Crude pirfenidone purity is >99,5% (HPLC analysis, UV detector 310 nm).

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 1003-68-5, 5-Methylpyridin-2(1H)-one.

Reference:
Patent; ULKAR KIMYA SANAYII VE TICARET A. S.; KOYUNCU, Hasan; AKGOL, Emre; REIS, Omer; (16 pag.)WO2016/122420; (2016); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 1003-68-5, 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. 1003-68-5, name is 5-Methylpyridin-2(1H)-one, molecular formula is C6H7NO, The 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.

5-methyl-2-pyridone (2) (20 g, 0,18 mol), K2C03 (30,4 g, 0,22 mol), NaOAc (3 g, 0,036 mol, 0,2 mol eq), CuBr (2,62 g, 0,018 mol, 0.1 mol eq) [or Cu20 (1 ,29 g, 0,05 mol eq)], Bromobenzene (4) (40,28 g, 0,26 mol, 1 ,4 mol eq) and DMSO (10 mL, 0,5 V eq) was placed in a round bottom flask under a nitrogen atmosphere. Flask was heated to 135-140C and stirred at this temperature for 6-8 h. After the completion of the reaction according to HPLC analysis, reaction medium was cooled down to about 60 C. Then, 100 mL water was added to the reaction mixture followed by 4 mL NH4OH and 100 mL toluene. The resulting mixture was stirred for 15 min and the phases were separated. Aqueous phase was extracted with 2×50 mL toluene then organic phases were combined (all extractions were carried out at about 60C). Combined organic phases were filtered over a bed of celite after treatment with charcoal. After evaporation of toluene to the dryness, 36,3 g crude pirfenidone was obtained. Crude pirfenidone purity is >99,5% (HPLC analysis, UV detector 310 nm).

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 1003-68-5, 5-Methylpyridin-2(1H)-one.

Reference:
Patent; ULKAR KIMYA SANAYII VE TICARET A. S.; KOYUNCU, Hasan; AKGOL, Emre; REIS, Omer; (16 pag.)WO2016/122420; (2016); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – 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. 1003-68-5, name is 5-Methylpyridin-2(1H)-one. A new synthetic method of this compound is introduced below., Quality Control of 5-Methylpyridin-2(1H)-one

General procedure: The coupling reaction was performed as follows: in a typical process, 5-methyl-2-(1H)-pyridone(1 mmol), aryl halide (1 mmol), base (2 mmol) and solvent (5 mL) were added to an oven-dried tube containing 5% (based on copper) MOF catalyst or copper salt. The mixture was stirred at desired temperature for 2 h. After being cooled to room temperature, the catalyst was filtrated and washed with ethyl acetate. The products were isolated by a series 1500 preparative high performance liquid chromatography system (SSI, Charlotte, NC, USA) equipped with a UV-VIS detector, using a Kromasil C18 column (50 x 250 mm) and gradient elution with a H2O (A)-acetonitrile (B) the mobile phase. The gradient program was 0 min, 10% B; 20 min, 35% B. The flow rate of mobile phase was 40 mL/min, and the detection wavelength was 220 nm. Fractions were collected and evaporated to afford the pure products.

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, 1003-68-5, 5-Methylpyridin-2(1H)-one.

Reference:
Article; Long, Wei; Qiu, Wenge; Guo, Chongwei; Li, Chuanqiang; Song, Liyun; Bai, Guangmei; Zhang, Guizhen; He, Hong; Kuznetsov, Maxim L.; Molecules; vol. 20; 12; (2015); p. 21178 – 21192;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 1003-68-5, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 1003-68-5, name is 5-Methylpyridin-2(1H)-one. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The coupling reaction was performed as follows: in a typical process, 5-methyl-2-(1H)-pyridone(1 mmol), aryl halide (1 mmol), base (2 mmol) and solvent (5 mL) were added to an oven-dried tube containing 5% (based on copper) MOF catalyst or copper salt. The mixture was stirred at desired temperature for 2 h. After being cooled to room temperature, the catalyst was filtrated and washed with ethyl acetate. The products were isolated by a series 1500 preparative high performance liquid chromatography system (SSI, Charlotte, NC, USA) equipped with a UV-VIS detector, using a Kromasil C18 column (50 x 250 mm) and gradient elution with a H2O (A)-acetonitrile (B) the mobile phase. The gradient program was 0 min, 10% B; 20 min, 35% B. The flow rate of mobile phase was 40 mL/min, and the detection wavelength was 220 nm. Fractions were collected and evaporated to afford the pure products.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 1003-68-5, 5-Methylpyridin-2(1H)-one.

Reference:
Article; Long, Wei; Qiu, Wenge; Guo, Chongwei; Li, Chuanqiang; Song, Liyun; Bai, Guangmei; Zhang, Guizhen; He, Hong; Kuznetsov, Maxim L.; Molecules; vol. 20; 12; (2015); p. 21178 – 21192;,
Pyridine – Wikipedia,
Pyridine | C5H5N – 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. 1003-68-5, name is 5-Methylpyridin-2(1H)-one. A new synthetic method of this compound is introduced below., Recommanded Product: 5-Methylpyridin-2(1H)-one

EXAMPLE 1 5-Methyl-1-phenyl-2-(1H)-pyridone SPC3 A finely pulverized mixture containing 21.8g. of 5-methyl-2-(1H)-pyridone (J.V. Scudi, et al. U.S. Pat. No. 2,947,755), 30.4g. of anhydrous potassium carbonate, 0.25g. of zinc precipitated copper powder and 40 ml. of iodobenzene is stirred mechanically and refluxed for 18 hours. The mixture is cooled and treated with 150 ml. of benzene, filtered and the filtrate is decolorized with charcoal. The decolorized benzene filtrate is then evaporated to an oil which on trituration with petroleum ether and cooling gives 31.9g. (85%) of the product as a brown solid, m.p. 90-104. It is crystallized from hot water to yield a white solid melting at 102-psi.

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, 1003-68-5, 5-Methylpyridin-2(1H)-one.

Reference:
Patent; Affiliated Medical Research, Inc.; US3974281; (1976); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 1003-68-5, 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 1003-68-5 as follows.

A mixture of Cul (0.19 g, 1 mmol), Cs2C03(6.85 g, 20 mmol) and ethyl 2-oxocyclohexanecarboxylate (0.34 g, 2 mmol) in DMSO (10 mL) was stirred at rt for 30 min under N2. Then to the reaction mixture was added a solution of 5-methylpyridone (1.09 g, 10 mmol) and 4-(2-fluoro-4-iodobenzyl) morpholine (3.21 g, 10 mmol) in DMSO (12 mL) via syringe. The reaction mixture was heated at 100 C overnight, cooled to rt and filtered. The filtrate diluted with H20 (50 mL) was extracted with CH2C12(50 mL x 3). The combined organic phases were concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE / EtOAc (V / V) = 10 : 1) to give the title compound as a white solid (0.70 g, 23%). The compound was characterized by the following spectroscopic data:MS (ESI, pos.ion) m/z: 303.2 (M+l);-NMR (400 MHz, CDC13): delta 2.06 (s, 3 H), 3.16-3.32 (m, 4 H), 3.86-3.97 (m, 4 H), 4.44 (s, 2 H), 6.47 (d, 1 H, J = 9.6 Hz), 7.39-7.44 (m, 2 H), 7.48 (s, 1 H), 7.52-7.55 (m, 1 H), 7.99 (t, 1 H, J= 8.2 Hz)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1003-68-5, its application will become more common.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; ZHANG, Yingjun; ZHANG, Jiancun; WANG, Xiaojun; LIN, Runfeng; CAO, Shengtian; WANG, Zhaohe; LI, Jing; WO2014/12360; (2014); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 1003-68-5, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 1003-68-5, name is 5-Methylpyridin-2(1H)-one. This compound has unique chemical properties. The synthetic route is as follows.

Sequentially adding to the reaction bottle 5-methyl -2 (1H)-pyridone 109 g, anhydrous potassium carbonate 165 g, cuprous bromide 0.72 g, bromophenylacetic 188.4 g, 1,10-phenan throline 0.9 g and N, N-dimethyl formamide 500 ml, the mixture is heated to 90 C about 2 hours, cooling to the end 25 C, by adding 2000 ml of water mixing, filtering, in the filter cake into the reaction bottle, by adding 5% acetic acid aqueous solution 1500 ml, the temperature is increased to 90 C, filtration, filtrate with 20% sodium hydroxide solution to adjust the pH= 13, and then cooled to the 5 C the following filtering, decompression drying to obtain the pirfenidone 132.5 g, spare.

According to the analysis of related databases, 1003-68-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Chongqing Kangle Pharmaceutical Co., Ltd; Tang, Ming; Chen, Wenhui; Chen, Lin; Ma, Xiaoping; Zheng, Xue; Yang, Jibin; Cai, Zhongwen; Wang, Yachuan; (6 pag.)CN105315198; (2016); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 1003-68-5, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 1003-68-5, name is 5-Methylpyridin-2(1H)-one. This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 21 1-(2’Imidazolyl)-5-methyl-2-(1H)-pyridone Following essentially the general procedure outlined in Example 1, the reaction of 5-methyl-2-(1H)-pyridone with 2-chloroimidazole affords 1-(2′-imidazolyl)-5-methyl-2-(1H)-pyridone in 82% yield.

According to the analysis of related databases, 1003-68-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Affiliated Medical Research, Inc.; US3974281; (1976); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – 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. 1003-68-5, name is 5-Methylpyridin-2(1H)-one. A new synthetic method of this compound is introduced below., Recommanded Product: 5-Methylpyridin-2(1H)-one

To a 25 mL round bottom flask was added 0.10 g (1 mmol, 1 quiv.) Of compound 3, 0.17 g (1 mmol, 1 quiv.) Of p-bromobenzaldehyde, 1.4 g (10 mmol, 10 equiv.) Of K2CO3,0.05 g (0.26 mmol, 0.26 equiv.) CuI,5 mL of DMF as solvent,Reflux stirring reaction 1h,TLC, the reaction was completed, the mixture was cooled, the mixture was extracted with 30 mL of water and extracted with 3 x 20 mL of ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, spin dried and separated by 300 mesh silica gel column chromatography. Eluent petroleum ether: ethyl acetate = : 3 (v / v) to give pale yellow solid: Compound 4.

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, 1003-68-5, 5-Methylpyridin-2(1H)-one.

Reference:
Patent; Sichuan Univeristy; Yi, Shufan; Li, Yong; Cao, Tingting; Yang, Ziyao; (17 pag.)CN106083702; (2016); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 1003-68-5, 5-Methylpyridin-2(1H)-one, 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, Recommanded Product: 1003-68-5, blongs to pyridine-derivatives compound. Recommanded Product: 1003-68-5

5-Methyl-2(1H)-pyridinone (50 g, 0.46 mol) was suspended in dichloromethane (500 mL). N-bromosuccinimide (82 g, 0.46 mol) was added in portions with cooling. Addition was finished after 15 min; the mixture was stirred for 1 h at room temperature and afterwards partitioned between dichloromethane and water. Organic phases were pooled, dried with Na2SO4 and the solvent was evaporated. The residue was purified by crystallization from ethyl acetate to yield 55 g of the title compound as a light yellow solid, mp 156-161 C.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1003-68-5, 5-Methylpyridin-2(1H)-one, and friends who are interested can also refer to it.

Reference:
Patent; Andjelkovic, Mirjana; Benardeau, Agnes; Chaput, Evelyne; Hebeisen, Paul; Nettekoven, Matthias; Sander, Ulrike Obst; Panousis, Constantinos G.; Roever, Stephan; US2008/85906; (2008); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem