Month: August 2021

Adding a certain compound to certain chemical reactions, such as: 16498-81-0, 2-Methoxynicotinic acid, 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, COA of Formula: C7H7NO3, blongs to pyridine-derivatives compound. COA of Formula: C7H7NO3

Step 2 Preparation of N-[2-(7,8-Dimethyl-2,4-dioxo-3,4-dihvdro-2H-benzo[glpteridin- 10-vD-ethyll-2-methoxy-nicotinamide; [0116] 2-Methoxy-nicotinic acid (20 mg, 0.12 mmol) and Hunig’s base (0.024 mL,0.14 mmol) are dissolved in DMF (1 mL) followed by addition of HATU (53 mg, 0.14 mmol) at room temperature and is stirred for one hour. 10-(2-Amino-ethyl)-7,8-dimethyl- 10H-benzo[g]pteridine-2,4-dione (39 mg, 0.14 mmol) (see Intermediate 1 for preparation) is dissolved in DMF (ImL) and added to the reaction mixture. After 3 h the reaction mixture is diluted with water (2 mL) and purification is performed using preparatory HPLC (Method 3). 3-[2-(7,8-Dimethyl-2,4-dioxo-3,4-dihydro-2H-benzo[g]pteridin-10- yl)-ethylamino] -benzoic acid (12 mg) is isolated following lyophilization of the appropriate fractions (Yield: 24%). 1H NMR (400 MHz, DMSO-d6) delta 11.37 (s, 1H), 8.48 (m, 1H), 8.28 (m, 1H)5 8.02 (m, 1H), 7.89 (m, 2H), 4.81 (m, 2H), 3.78 (m, 5H), 2.33 (s, 3H), 2.30 (s, 3H). LC-MS m/z 421.2 [M+H]+. Retention time = 5.31 min.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,16498-81-0, 2-Methoxynicotinic acid, and friends who are interested can also refer to it.

Reference:
Patent; BIORELIX, INC.; COISH, Philip, D.G.; WICKENS, Philp; AVOLA, Stephanie; BABOULAS, Nick; BELLO, Angelica; BERMAN, Judd; KAUR, Harpreet; MOON, David; PHAM, Vinh; ROUGHTON, Andrew; WILSON, Jeffrey; ARISTOFF, Paul, Adrian; BLOUNT, Kenneth, F.; DIXON, Brian, R.; MYUNG, Jayhyuk; OSTERMAN, David; BELLIOTTI, Thomas, R.; CHRUSCIEL, Robert, A.; EVANS, Bruce, R.; LEIBY, Jeffrey, A.; SCHOSTAREZ, Heinrich, J.; UNDERWOOD, Dennis; NAVIA, Manuel; SCIAVOLINO, Frank; WO2011/8247; (2011); 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. 14254-57-0, name is Isonicotinoyl chloride, molecular formula is C6H4ClNO, 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. Application In Synthesis of Isonicotinoyl chloride

General procedure: 1 equiv of cinnamamide was dissolved in dry DCM followed byaddition of 3 equiv of Et3N and stirred at 0 C under inert atmosphere.1.5 equiv of isonicotinoyl chloride dissolved in DCM wasdirectly added dropwise to above stirred solution at 0 C. The reactionmixture was stirred for 0.5 h. The reaction progress was monitoredby TLC. After completion of the reaction, the reaction mixturewas diluted with water (30 ml) and extracted with DCM twice. Theorganic layer was washed successively with saturated bicarbonatesolution (220 ml) and brine solution (20 ml). The organic layerwasdried over anhydrous sodium sulfate and was evaporated underreduced pressure. The crude product was recrystallized from ethylacetate and hexane to afford the desired product.

With the rapid development of chemical substances, we look forward to future research findings about 14254-57-0.

Reference:
Article; Patel, Kavitkumar N.; Telvekar, Vikas N.; European Journal of Medicinal Chemistry; vol. 75; (2014); p. 43 – 56;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 1121-19-3, 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. 1121-19-3, name is 4-Methylpyridin-3-ol, 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.

4-Methylpyridin-3-ol (5.00 g, J. Heterocyclic Chem. , 1985, 22, 1419) was added to cone. H2SO4 (25 mL) under ice- cooling (below 300C). Nitric acid (fuming, 2.2 mL) was added dropwise below 100C, and the mixture was stirred at 10-200C for 2 hr and then poured onto crashed ice. The mixture was adjusted to pH 2 by the addition of 8N NaOH and extracted with ethyl acetate (2 x) . The extracts were combined, dried over MgSO4 and concentrated, and the residue was chromatographed on silica gel using n-hexane/ethyl acetate as an eluent to give the title compound as yellow crystals (4.89 g) . mp. 87-880C.1H-NMR (300 MHz, DMSO-d6) delta: 2.31 (s, 3H), 7.56 (d, J = 4.2 Hz, IH), 7.93 (d, J = 4.2 Hz, IH), 10.55 (br, IH).

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 1121-19-3, 4-Methylpyridin-3-ol.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2007/77961; (2007); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – 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. 68470-59-7, name is 2-(Bromomethyl)-6-methylpyridine. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 68470-59-7

(2.0 g, 11.35 mmol), potassium carbonate (2.4 g, 17.03 mmol) and Ib (2.2 g, 11.92 mmol) were added to DMF (20 mL), respectively, and stirred overnight at room temperature.The reaction was poured into water and extracted with EtOAc (100 mL x 2).The organic phase was washed with water and saturated brine, and dried over sodium sulfate.After filtration, the filtrate was concentrated and separated by column chromatography (EtOAc / Pet. Ether, 1/10 to 1/4, v / v) to give the product as pale white solid 1c (1.6 g, 50%)

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, 68470-59-7, 2-(Bromomethyl)-6-methylpyridine.

Reference:
Patent; Suzhou Xiangshi Pharmaceutical Development Co., Ltd; Bu, Xianyong; Yuehan, Fuchuier; Andongni, Kuzubi; Wu, Leguang; Liu, Shiqiang; (30 pag.)CN105985322; (2016); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 717106-69-9, Methyl 2-(6-chloropyridin-3-yl)acetate, 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, Product Details of 717106-69-9, blongs to pyridine-derivatives compound. Product Details of 717106-69-9

General procedure: To a solution of 1,4-dibromobutane (4.88g, 22.5mmol) and methyl 2-(6-chloropyridin-3-yl)acetate (2.79g, 15.0mmol) in THF (150mL) was added a 1.0M solution of LHMDS in THF (18.8mL, 18.8mmol) dropwisely at 0C. The reaction mixture was stirred at rt for 2.0h, then was added a 1.0M solution of LHMDS in THF (18.8mL, 18.8mmol) slowly at rt. The reaction mixture was stirred at rt overnight, quenched with brine, and extracted with ethyl acetate (30mL, 3×). The combined organic layers were dried (MgSO4) and concentrated under reduced pressure. The resulting residue was purified by column chromatography with pre-packed silica gel disposable column to afford the title compound 2a (2.26g, 63%) as a white solid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,717106-69-9, Methyl 2-(6-chloropyridin-3-yl)acetate, and friends who are interested can also refer to it.

Reference:
Article; Zhang, Dehui; Zheng, Hongchao; Wang, Xiaodong; Tetrahedron; vol. 72; 16; (2016); p. 1941 – 1953;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 83004-13-1, 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 83004-13-1, name is 2-Bromo-6-ethylpyridine. This compound has unique chemical properties. The synthetic route is as follows.

b 2-Bromo-6-ethyl-pyridine 1-oxide To a solution of 2-bromo-6-ethyl-pyridine (15.4 g, 82.8 mmol) (S. G. Davies and M. R. Shipton, J. Chem. Soc., Perkin Trans. 1, 1991, 3, 501) in acetic acid (15 ml) was added peracetic acid (26 ml of a 39percent solution) maintaining T<50° C. After complete addition the mixture was stirred at 50° C. for 5 hr and then cooled to room temperature (rt). Crushed ice (40 g) was added and the pH was adjusted to pH 12 with 40percent aqueous KOH solution. After extraction with CHCl3 (6*60 ml) the combined organic phases were dried (Na2CO3) and evaporated to give 20.0 g (>100percent) of the title compound, MS: m/e=201 (M+) as a yellow oil.

According to the analysis of related databases, 83004-13-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Alanine, Alexander; Buettelmann, Bernd; Heitz Neidhart, Marie-Paule; Pinard, Emmanuel; Wyler, Rene; US2003/119870; (2003); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 1597-32-6, 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. 1597-32-6, name is 2-Amino-6-fluoropyridine. A new synthetic method of this compound is introduced below.

To a solution of 4-cyanothiazole-2-carboxylic acid 15(30.0mg, 0.19 mmol) and N-methylmorpholine(60.0 muL, 0.53 mmol) in THF (5.0 mL) at -78C, isobutyl chloroformate (28.0 muL, 0.21 mmol) was added. The mixture was stirred at -5 C for 1 hour and a solution of2-amino-6-fluoropyridine (92.0 mg, 0.82 mmol) in THF (2.0 mL) was added. The mixture was stirred at room temperature overnight. The subsequent solution wasconcentrated under reduced pressure, extracted with H2O/ethylacetate and washed with HCl 1M. The combined organic layer was dried over Na2SO4, concentrated under reduced pressure and purified by column chromatography on silica gel using (hexane/ ethyl acetate = 3:1,) to afford N-(6-fluropyridin-2-yl)-4-cyanothiazole-2-carboxamide 6ce (20.0 mg, 41%) as pale yellow solid: 1H-NMR (400 MHz, CDCl3) delta 9.44 (s, 1H), 8.28 (s, 1H), 8.16-8.13 (dd, J = 7.80, J= 1.76, 1H), 7.91-7.85 (dd, J = 8.00, J = 16.0, 1H), 6.79-6.76 (dd, J= 8.00, J = 2.35, 1H). 13C-NMR(100 MHz, CDCl3) delta 164.5, 163.3, 160.9, 156.0,148.2, 148.1, 143. 6, 143.5, 135.8, 127.8, 112.8, 110.8, 110.77, 106.0, 105.7.LC/MS (ESI-) 246.9 (M-H)+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1597-32-6, 2-Amino-6-fluoropyridine, and friends who are interested can also refer to it.

Reference:
Article; Vu, Hoang Nam; Kim, Ji Young; Hassan, Ahmed H.E.; Choi, Kihang; Park, Jong-Hyun; Park, Ki Duk; Lee, Jae Kyun; Pae, Ae Nim; Choo, Hyunah; Min, Sun-Joon; Cho, Yong Seo; Bioorganic and Medicinal Chemistry Letters; vol. 26; 1; (2016); p. 140 – 144;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 80194-68-9, 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. 80194-68-9, name is 3-Chloro-5-(trifluoromethyl)picolinic acid. A new synthetic method of this compound is introduced below.

(1) Add 1 g (1 mmol) of 3-chloro-5-trifluoromethylpicolinic acid and 5 ml of a solvent to a 50 ml single-neck round bottom flask,Add a few drops of the DMF mixture and stir for 10 min.Slowly add a mixture of 0.675 g (1.2 mmol) of oxalyl chloride and DCM. After the dropwise addition, stir at room temperature for 3 h and stop the reaction.The system was spin-dried to obtain intermediate 2;

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,80194-68-9, its application will become more common.

Reference:
Patent; Guizhou University; Xu Fangzhou; Wu Jian; Luo Dexia; Guo Shengxin; He Feng; Zhang Renfeng; Chen Shunhong; (29 pag.)CN110526863; (2019); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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 66572-56-3, name is 2-Bromoisonicotinic acid. This compound has unique chemical properties. The synthetic route is as follows. Quality Control of 2-Bromoisonicotinic acid

At 20 C,5.0 g of 2-bromopyridine-4-carboxylic acid (24.9 mmol, 1.0 eq), 4.46 g of CuCN (49.8 mmol, 2.0 eq), 50 mL of DMF was added to a 100 mL single-mouth bottle, replaced with nitrogen three times, and heated in an oil bath at 120 C for 18 h. The heating was stopped, cooled to room temperature, and most of the DMF was removed by rotary evaporation, poured into water, extracted with EA 200 mL three times, and the organic phase was washed twice with 50 mL of water and 20 mL of saturated sodium chloride. The organic phase is dried and dried to give a crude product. 2.0g crude product as a white solid after recrystallization from methanol,Yield: 54.2%.

With the rapid development of chemical substances, we look forward to future research findings about 66572-56-3.

Reference:
Patent; Jinan Shaoyuan Pharmaceutical Co., Ltd.; Shaoyuan Science And Technology (Shanghai) Co., Ltd.; Wang Haibo; Pan Tingting; Zheng Yan; (7 pag.)CN109836379; (2019); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem