Day: December 23, 2020

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 769-28-8, name is 4,6-Dimethyl-2-oxo-1,2-dihydropyridine-3-carbonitrile. This compound has unique chemical properties. The synthetic route is as follows. Computed Properties of C8H8N2O

Add 5.0g (0.034mol) to a 500mL single-mouth bottle4,6-dimethyl-3-cyanopyrimidin-2-one,250mL of methanol, not fully soluble,25mL 25% ammonia water,About 5.0g of nickel, replaced by argon three times,The hydrogen was replaced three times, and the temperature was raised to 50 C. After 11 h of reaction, the TLC reaction was complete.Stop the reaction and filter the solution through diatomaceous earth.The filtrate was evaporated to dryness to give 6.3 g, m.Dissolve the product with methanol,Placed in an ice salt bath,20mL of 4N hydrochloric acid ethanol solution was added dropwise with stirring.After the drop,After stirring for 1 h in an ice bath, a large amount of white solid was precipitated, which was filtered with suction to give a white solid.Wash twice with ethanol, suction filtration,Dry to give 5.0 g of a white solid.The yield was 96.9%.

With the rapid development of chemical substances, we look forward to future research findings about 769-28-8.

Reference:
Patent; Shenyang Pharmaceutical University; Chen Guoliang; Wang Lihui; Zhou Qifan; Du Fangyu; Dong Xiaoyu; Yang Jingyu; Wu Chunfu; (48 pag.)CN109320499; (2019); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.153034-86-7, name is 2-Chloro-4-iodopyridine, molecular formula is C5H3ClIN, molecular weight is 239.44, as common compound, the synthetic route is as follows.category: pyridine-derivatives

c) 2-Chloro-4-(5-methyl-3-phenyl-isoxazol-4-ylethynyl)-pyridine A mixture of 4-ethynyl-5-methyl-3-phenyl-isoxazole (110 mg, 0.60 mmol), 2-chloro-4-iodopyridine(172 mg, 0.72 mmol), triethylamine (209 mul, 1.50 mmol) and bis(triphenylphosphine)palladium(II) chloride (13 mg, 0.02 mmol) in N,N-dimethylformamide (1.2 mL) was evaporated and flushed with argon. Cuprous iodide (2 mg, 0.01 mmol) was added and the reaction mixture was stirred for 1.5 h at 90 C. before it was cooled to ambient temperature and separated between aqueous sodium hydroxide (1 M, 20 mL) and ethyl acetate (30 mL). The aqueous layer was extracted with ethyl acetate (30 mL) and the combined organic layers were washed with aqueous sodium hydroxide (1 M, 20 mL), dried over sodium sulfate and concentrated. Purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 80:20) afforded the title compound (160 mg, 91%) as a colorless oil. MS: m/e=295.0/297.2 [M+H]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,153034-86-7, 2-Chloro-4-iodopyridine, and friends who are interested can also refer to it.

Reference:
Patent; Buettelmann, Bernd; Knust, Henner; Thomas, Andrew; US2007/287739; (2007); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – 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. 19828-20-7, name is 2-Amino-5-acetylpyridine, molecular formula is C7H8N2O, 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. Quality Control of 2-Amino-5-acetylpyridine

Step A: 2-(6-Aminopyridin-3-yl)-6-chloroquinoline-4-carboxylic acid (27) [00392] A solution of l-(6-aminopyridin-3-yl)ethanone 16, example 8, step A) (1.5 g, 11.0 mmol) in ethanol (10 mL) was added slowly to a solution of 5-chloroindoline-2,3-dione (9) (1.66 g, 9.17mmol) in 6M aqueous KOH (lOmL) at 100C. The reaction was monitored by LCMS until the staring material consumed. Then the reaction mixture was concentrated to remove ethanol, the residue was diluted with water (10 mL), the pH value of the mixture was acidified to 5 by adding 1M aqueous HCl solution. The precipitate was filtered to give the desired product (1.2 g, 44%) as an orange solid. LC-MS: (M + H)+ 300.1

With the rapid development of chemical substances, we look forward to future research findings about 19828-20-7.

Reference:
Patent; NEW YORK UNIVERSITY; UNIVERSITY OF ALBANY; SCHMIDT, Ann, Marie; RAMASAMY, Ravichandran; SHEKHTMAN, Alexander; RAI, Vivek; MANIGRASSO, Michaele, B.; (179 pag.)WO2017/184547; (2017); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 960299-32-5, 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. 960299-32-5, name is 3-Bromo-6-chloro-1-methylpyridin-2(1H)-one. A new synthetic method of this compound is introduced below.

A mixture of 27.28 g of 3-bromo-6-chloro-1-methylpyridin-2 (1H) -one, 47.94 g of cesium carbonate and 100 mL of DMF was cooled with ice.19.32 g of 2,2,3,3,3-pentafluoro-1-propanol was added dropwise and stirred at room temperature for 3 hours. To the resulting mixture was added water and extracted with ethyl acetate. The obtained organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue obtained is washed successively with water and hexane and is shown below39.41 g of Intermediate A-28 was obtained.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,960299-32-5, 3-Bromo-6-chloro-1-methylpyridin-2(1H)-one, and friends who are interested can also refer to it.

Reference:
Patent; Sumitomo Chemical Co., Ltd.; Murakami, Shinichiro; (468 pag.)JP2019/65018; (2019); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 154078-83-8, Adding some certain compound to certain chemical reactions, such as: 154078-83-8, name is Ethyl 2-(3-nitropyridin-2-yl)acetate,molecular formula is C9H10N2O4, 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 154078-83-8.

c Ethyl 2-(3-Amino-pyridin-2-yl)-acetate Under an atmosphere of nitrogen, Pd/C (10%, 1.36 g) was added to a round bottom flask. Ethyl 2-(3-nitro-pyridin-2-yl)-acetate (8.6 g, 0.41 mol) was dissolved in ethanol (200 mL) and added to the reaction vessel. The reaction was placed under an atmosphere of hydrogen and stirred at room temperature for 30 min. The reaction was filtered through celite, and the filtrate was concentrated in vacuo to afford the title compound as a tan solid (6.94 g, 94% yield).

According to the analysis of related databases, 154078-83-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SmithKline Beecham Corporation; US6624171; (2003); B1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 141-86-6, name is 2,6-Diaminopyridine, the common compound, a new synthetic route is introduced below. Recommanded Product: 2,6-Diaminopyridine

Example 1 N, /V’-(pyridine-2, 6-diyl) dibenzamid 1) Synthetic Procedure: In a round bottom flask 2, 6-diaminopyridine (lg, 9.163 mmol) was dissolved in 40mL of dry dichloromethane and triethylamine (2.8mL, 27.72mmol) was added. Then, benzoyl chloride (2.5mL, 17.98 mmol) was added drop by drop and this mixture was stirred under inert atmosphere at room temperature for 15h. Reaction mixture was poured in water. Crude product was extracted in dichloromethane, organic layer was washed with water and dried over anhydrous sodium sulphate. The solvent was evaporated on rotary evaporator and crude product was purified by column chromatography on silica gel by eluting with ethyl acetate: hexane (40:60) mixture. The product was further purified by recrystallization using a methanol. Yield: 2.60 g (89%). NMR (200MHz, CDC13): delta ppm 7.54 (m, 6H), 7.90 (d, 4H, J=6Hz), 7.82 (t, 1H, J=8Hz), 8.10 (d, 2H, J=8Hz), 8.39 (s, 2H).

The synthetic route of 141-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH; AMBADE, Ashootosh Vasant; PESALA, Bala; JOSHI, Kavita; BASUTKAR, Nitin Bapurao; RAY, Shaumik; DASH, Jyotirmayee; VILASRAO, Kaware Vaibhav; WO2015/104722; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 78607-36-0, 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 78607-36-0 as follows.

To a THF solution (40 ml) of Diisopropyl amine (4.46 ml, 1.5 eqv) was added BuLi (1.88 M, 1.5 eqv) at -15 C. and the resulting reaction mixture was allowed to stir at same temperature for 20 minutes. It was then cooled to -78 C. and 2-chloro-3-iodopyridine (5 g, 20.92 mmol) in THF (10 ml) was added dropwise at the same temperature and allowed to stir for 1 hr at -78 C. Reaction was quenched with water (10 ml), stirred at ambient temperature for 15 minutes and extracted with ethyl acetate. Organic layer was washed successively with brine and finally dried over sodium sulfate. Evaporation of organic layer under reduced pressure gave the crude product which was immediately used in the next step without any further purification. Yield: 80% (Crude)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,78607-36-0, its application will become more common.

Reference:
Patent; GRUENENTHAL GmbH; US2009/186899; (2009); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 105170-27-2, 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. 105170-27-2, name is 2-Bromo-5-methoxypyridine, molecular formula is C6H6BrNO, 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.

General procedure: A mixture of 2-Bromo-5-methoxypyridine 1 (2.82 g, 15 mmol), copper iodide (286mg, 1.5 mmol, 10 mol%), diisopropylethylamine (3.14 ml, 18 mmol) and bis(triphenylphosphine) palladium chloride (316 mg, 0.45 mmol, 3 mol%) in dimethylformamide (30 ml) at r.t. was evacuated then back filled with nitrogen. Triethylsilylacetylene(3.22 ml, 18 mmol) was added and the resulting mixture was stirred at r.t. for 24 hours. The crude reaction mixture was then diluted with ethyl acetate (100ml) and washed with water (2×30 ml), brine (30 ml), dried over sodium sulfate, filtered and concentrated to an oil. The oil was purified by flash chromatography using an ISCO 80g column eluting with a gradient of 0 to 30% EtOAc in heptane to give 3.53 g of 5-methoxy-2-triethylsilanylethynylpyridine 2 as an amber oil. LCMS-ESI(+): [MH]+=248;1H NMR (400MHz, CHLOROFORM-d) d= 8.27 (d, J=3.0 Hz, 1H), 7.42 (d, J=8.6 Hz, 1H), 7.13 (dd, J=3.0,8.6 Hz, 1H), 3.87 (s, 3H), 1.06 (t, J=7.8 Hz, 9H), 0.70 (q, J=7.8Hz, 6H)

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 105170-27-2, 2-Bromo-5-methoxypyridine.

Reference:
Article; Braganza, John F.; Bernier, Louise; Botrous, Iriny; Collins, Michael R.; Li, Baohua; McAlpine, Indrawan; Ninkovic, Sacha; Ren, Shijian; Sach, Neal; Tran-Dube, Michelle; Zeng, Qingbin; Zheng, Baojiang; Tetrahedron Letters; vol. 56; 42; (2015); p. 5757 – 5760;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 911434-05-4, 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 911434-05-4, name is 5-Bromo-2-methyl-3-nitropyridine. This compound has unique chemical properties. The synthetic route is as follows.

A mixture of T-3 (13.2 g, 60.8 mmol) and iron powder (11.50 g, 205.9 mmol) in acetic acid (150 mL) is warmed at reflux. After 2 hours, the reaction is diluted with Et2O (100 mL) and EtOAc (250 mL) and filtered through filter agent washing with ethyl acetate. The filtrate is diluted with water (200 mL) made basic with first K2CO3 and then NaHCO3 and extracted with EtOAc (3 x 150 mL). The combined organic layers are washed with saturated aqueous NaHCO3 (100 mL), brine (2 x 100 mL), dried over magnesium sulfate, filtered and concentrated to provide T-4.

According to the analysis of related databases, 911434-05-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BETAGERI, Rajashekhar; COOK, Brian, Nicholas; DISALVO, Darren; HARCKEN, Christian; KUZMICH, Daniel; LIU, Pingrong; LORD, John; MAO, Can; RAZAVI, Hossein; WO2012/87782; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.54189-82-1, name is 6-Chloro-N-methylnicotinamide, molecular formula is C7H7ClN2O, molecular weight is 170.6, as common compound, the synthetic route is as follows.category: pyridine-derivatives

6-({2-[(2/?,5/?)-2>5-dimethyl-1-pyrrolidinyl]-2,3-dihydro-1H-inden-5-yl}oxy)-yV-methyl- 3-pyridinecarboxamide (E9) Sodium hydride (22mg, 0.55mmol, 60% in mineral oil) was added to a solution of 2-[(2f?,5R)-2,5-dimethyl-1-pyrrolidinyl]-2,3-dihydro-1H-inden-5-ol (may be prepared as described in Description 8) (105mg, 0.45mmol) in dimethylformamide (4ml) and the resulting mixture was stirred at room temperature for 20 minutes. 6-Chloro-Lambda/-methyl-3- pyridinecarboxamide (93mg, 0.55mmol; may be prepared as described in Description 10 of WO2004056369) was added and the mixture heated at 9O0C under argon for 21 hours. The mixture was then cooled to room temperature, applied to an sex ion exchange column and eluted with methanol and then a solution of ammonia in methanol (2M). The basic fractions were evaporated under reduced pressure and the residue purified on the mass directed autoprep to afford the title compound (E9); MS (ES+) m/e 366 [M+H]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,54189-82-1, 6-Chloro-N-methylnicotinamide, and friends who are interested can also refer to it.

Reference:
Patent; GLAXO GROUP LIMITED; WO2006/61193; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem