Day: April 8, 2022

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. 13466-35-8, name is 3-Chloro-2-hydroxypyridine, the common compound, a new synthetic route is introduced below. name: 3-Chloro-2-hydroxypyridine

Chlorination: 40 g of 3-chloro-2-hydroxypyridine and 100 g of dichloroethane,DMF0.3g,Phosphorus oxychloride 56g was added to the reaction flask and refluxed.In the control,After the reaction is over,Distilled ethylene dichloride,Slowly add cold water to the reaction solution.After fully hydrolyzing, adjust the pH to 4-5 and steam it.Get 2,3-dichloropyridine,Dry at room temperature and dry at 43gThe purity is 99.1%.

The synthetic route of 13466-35-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhou Kaiyuan People’s Welfare Technology Co., Ltd.; Zhao Fei; Song Liang; Chen Wei; Wei Haihao; Zeng Miao; Xu Jianfeng; (8 pag.)CN107935921; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 69045-78-9 ,Some common heterocyclic compound, 69045-78-9, molecular formula is C6H3Cl4N, 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.

The obtained 2-chloro-5-trichloromethylpyridine 46.2 g,After adding the catalyst, the temperature is raised to 150-160C.Slowly dry the chlorine gas for heavy chlorination.After 6 hours of reaction, dilute the reaction solution with benzene, wash with water and dry the organic phase.After evaporating the benzene under reduced pressure,After distillation, 50.3 g of oily product was obtained.That is the intermediate 2,3-dichloro-5-trichloromethylpyridine,The yield was 90% and the content was 95%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,69045-78-9, its application will become more common.

Reference:
Patent; Shandong Eastern Countries Nong Pharmaceutical Ji Industrial Co., Ltd.; Yu Lexiang; Li Yuan; Liu Weihua; Sun Meixin; Sun Fujiang; (7 pag.)CN106748985; (2017); 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. 131747-62-1, name is 3-(Trifluoromethyl)pyridine-2-carboxaldehyde. A new synthetic method of this compound is introduced below., SDS of cas: 131747-62-1

To a solution of 185 (50 mg, 0.2808 mmol) in toluene 15 ml was added 66 (68.8 mg, 0.393 mmol). PTSA (106.7 mg, 0.561 mmol) was added to the reaction mass and stirred at 120 C. for 6 h. The reaction mass was diluted with ethyl acetate and washed with water (3×25 ml.). The organic layer was dried over sodium sulphate and concentrated to get the crude 189, which was used for next step without further purification.

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, 131747-62-1, 3-(Trifluoromethyl)pyridine-2-carboxaldehyde.

Reference:
Patent; Vankayalapati, Hariprasad; Yerramreddy, Venkatakrishnareddy; US2015/72980; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 28733-43-9 , The common heterocyclic compound, 28733-43-9, name is 5-Bromonicotinamide, molecular formula is C6H5BrN2O, 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.

Step 1: 3-Amino-5-bromopyridine To a ice-cold solution of 31.8 g (0.79 mol) of Sodium hydroxide and 40.7 g (0.255 mol) of Bromine in 340 ml of water were added 42.0 g (0.209 mol) of commercially available 5-Bromonicotinamide. The mixture was allowed to warm up to room temperature and then heated for 1 h at 70 C. The resulting brown suspension was allowed to cool to room temperature. The aqueous phase was saturated with brine and extracted three times with a 1:1 mixture of THF and t-Butyl-methyl ether. The combined organic phases were dried over magnesium sulfate, filtered and concentrated in vaccuo. Concentration in vaccuo yielded 39.1 g of a dark brown residue which was purified by flash chromatography (heptane/ethyl acetate 1:1) to yield the title compound as a brown solid (total 70.2 g, 70%), MS (ISP): m/e=173.1, 175.1 (M+H+).

The synthetic route of 28733-43-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jaeschke, Georg; Kolczewski, Sabine; Porter, Richard Hugh Philip; Vieira, Eric; US2006/199960; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 75806-86-9 ,Some common heterocyclic compound, 75806-86-9, molecular formula is C5H2BrClN2O2, 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.

To a solution of sodium hydride [(1 .52 g, 63.17 mmol (95%)] in DMSO (20.0 mL) at 0 00 diethylmalonate (10.11 g, 63.17 mmol) was added and kept for reflux at 100 00for 1 h. The reaction mixture was cooled to room temperature before drop wise addition of intermediate 32b (10.0 g, 42.11 mmol) in DMSO (20 mL) . The resultingmixture wasrefluxed at 100 00 for 3 h. The reaction mixture was quenched with ice water and extracted by using Ethyl acetate washed with water, and dried over anhydrous Na2SO4. The solvent was removed under vacuo to yield the title compound (10.0 g, 75.00%) as a brown oily product. LOMS: (M-H) = 315.0

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. 75806-86-9, 2-Bromo-5-chloro-3-nitropyridine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; MADANAHALLI RANGANATH RAO, Jagannath; GURRAM RANGA, Madhavan; PACHIYAPPAN, Shanmugam; WO2014/202528; (2014); 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. 89364-04-5, name is 3-Bromo-4-nitropyridine. A new synthetic method of this compound is introduced below., Recommanded Product: 89364-04-5

DMF (100 mL) was degased by vacuum/nitrogen filling cycles. 3-Bromo-4-nitropyridine (4.01 g, 19.74 mmol), 5-(4,4,5,5-tetramethyl-1 ,3,2-dioxaborolan-2-yl)thiazole (5 g, 23.69 mmol), cesium fluoride (7.50 g, 49.3 mmol), copper(l) iodide (0.376 g, 1.974 mmol) and Pd(Ph3P)4 (1.140 g, 0.987 mmol) were added and the crude was heated at 90C for 18 h. The reaction was cooled to room temperature and diluted with ethyl acetate. The organic phase was washed several times with water and brine, dried over Na2S04, filtered and concentrated under reduced pressure. The residue was purified by chromatography on silica using a Biotage Isolera system employing dichloromethane/methanol (98/2) to afford the desired product (3.80 g, 93 %). (0176) 1H NMR (400 MHz, DMSO-d6) d 9.32 (s, 1 H), 9.02 (s, 1 H), 8.96 (d, 1 H), 8.16 (s, 1 H), 8.08 (d, 1 H).

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, 89364-04-5, 3-Bromo-4-nitropyridine.

Reference:
Patent; AC IMMUNE SA; LIFE MOLECULAR IMAGING SA; BERNDT, Mathias; MUeLLER, Andre; ODEN, Felix; SCHIEFERSTEIN, Hanno; SCHMITT-WILLICH, Heribert; KROTH, Heiko; MOLETTE, Jerome; (49 pag.)WO2019/145291; (2019); A1;,
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. 73583-41-2, name is 4-Bromo-3-chloropyridine. This compound has unique chemical properties. The synthetic route is as follows. Formula: C5H3BrClN

Step 2: N1-(3-chloropyridin-4-yl)-N2-(2-((7-chloroquinolin-4-yl)amino)ethyl)-N2- methylethane- 1 ,2-diamine [00252] A mixture of 4-bromo-3-chloropyridine (0.171 g, 0.886 mmol), N1-(2-aminoethyl)- N2-(7-chloroquinolin-4-yl)-N1-methylethane-l,2-diamine (0.247 g, 0.886 mmol), Pd(OAc)2 (22 mg), BINAP (0.12 g), and K3P04 (1.0 g) in 1,4-dioxane (8.9 mL) was degassed with argon for 5 min and then stirred at 100 C for 16.5 h in a sealed tube. The reaction mixture was cooled to room temperature, filtered through Celite, and concentrated in vacuo. Purification by silica gel chromatography using CH2Cl2/CH3OH/NH4OH (270:9: 1, and 180:9: 1) afforded N1-(3-chloropyridin-4-yl)-N2-(2-((7-chloroquinolin-4-yl)amino)ethyl)-N2- methylethane-l,2-diamine (0.276 g, 80%) as a pale-yellow oil, and further lyophilization with CH3CN/H20 gave an off-white solid. 1H NMR (300 MHz, DMSO-d6) delta 2.32 (s, 3H); 2.66 (t, J = 6.3, 2H); 2.72 (t, J = 6.6, 2H); 3.26 (q, J = 5.7, 2H); 3.40 (q, J = 6.0, 2H); 6.04 (t, J = 5.0, 1H); 6.50 (d, J = 5.4, 1H); 6.64 (d, J = 5.7, 1H); 7.24 (t, J = 4.8, 1H); 7.43 (dd, J = 2.1, 9.0, 1H); 7.78 (d, J = 2.1, 1H); 8.02 (d, J = 5.7, lH); 8.11 (s, 1H); 8.20 (d, J = 9.3, 1H); 8.38 (d, J = 5.4, 1H). Mass spectrum (ESI) m/e = 390.1 (M+l).

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, 73583-41-2, 4-Bromo-3-chloropyridine.

Reference:
Patent; PRESAGE BIOSCIENCES, INC.; DECKWERTH, Thomas; KLEINMAN, Edward; RUAN, Fuqiang; BAKER, William; KLINGHOFFER, Richard; (126 pag.)WO2016/196393; (2016); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 56826-61-0, 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 56826-61-0 as follows.

A mixture of the 3-hydroxymethyl-2-methylpyridine (9.Og, 73.1mmol) and manganese (IV) dioxide (28. Ig, 322mmol) in DCM (100ml) was heated at reflux for two days. The insolubles were removed by filtration through diatomaceous earth and the filter pad was washed with methanol / DCM. The solvent was removed from the filtrate by evaporation to give 2-methylrhoyridine-3-carboxaldehyde (7.5g, 85%) as an oil; NMR Spectrum 2.78 (s, 3H), 7.43 (dd, IH), 8.15 (dd, IH), 8.66 (dd, IH).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,56826-61-0, its application will become more common.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/100461; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 100114-58-7, 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. 100114-58-7, name is 4-Amino-2-(hydroxymethyl)pyridine, molecular formula is C6H8N2O, 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.

Methyl 3-chloro-l-methyl-4-[[(lR)-2,2,2-trifluoro-l-methyl-ethyl]sulfamoyl]pyrrole-2- carboxylate (400 mg, 0.57 mmol) and (4-aminopyridin-2-yl)methanol (157 mg, 1.26 mmol) were dissolved in dry THF (5 mL). Lithium bis(trimethylsilyl)amide (1M in THF) (3.4 mL, 1 M, 3.4 mmol) was added drop wise and the reaction mixture was stirred overnight at room temperature. The reaction mixture was next quenched with sat. NH4C1 (10 mL). The organic layer was removed and the aqueous layer extracted with CH2CI2 (2 X 5 mL). The combined organic layers were evaporated to dryness and the residue was purified on silica using a heptane to EtOAc gradient yielding 3-chloro-N-[2-(hydroxymethyl)-4-pyridyl]-l-methyl-4-[[(lR)-2,2,2- trifluoro-l-methyl-ethyl]sulfamoyl]pyrrole-2-carboxamide (249 mg) as an off-white powder after trituration with diisopropylether. Method B: Rt: 0.81 min. m/z: 439 (M-H)” Exact mass: 440.1. 1H NMR (400 MHz, DMSO-d6) 5 ppm 1.19 (d, J=7.0 Hz, 3 H), 3.78 (s, 3 H), 3.92 – 4.05 (m, 1 H), 4.53 (d, J=5.7 Hz, 2 H), 5.42 (t, J=5.8 Hz, 1 H), 7.55 (dd, J=5.5, 2.0 Hz, 1 H), 7.68 (s, 1 H), 7.79 (d, J=1.5 Hz, 1 H), 8.38 (d, J=5.5 Hz, 1 H), 8.50 (br. s., 1 H), 10.69 (s, 1 H). DSC: From 30 to 300 C at 10C/min, peak 233.9 C. 3-chloro-N-[2-(hydroxymethyl)-4-pyridyl]-l- methyl-4-[[(lR)-2,2,2-trifluoro-l-methyl-ethyl]sulfamoyl]pyrrole-2-carboxamide (181 mg, 0.41 mmol) was dissolved in THF (5 mL). (Diethylamino)sulfur trifluoride (108.5 mu, 0.82 mmol) was added and the reaction mixture was stirred overnight at room temperature. The volatiles were removed under reduced pressure and the residue was purified via prep. HPLC (Stationary phase: RP XBridge Prep C18 OBD-IotaOmicronmuiotaeta, 30x150mm, Mobile phase: 0.25% (0700) NH4HCO3 solution in water, MeOH) yielding 3-chloro-N-[2-(fluoromethyl)-4-pyridyl]-l- methyl-4-[[(lR)-2,2,2-trifluoro-l-methyl-ethyl]sulfamoyl]pyrrole-2-carboxamide (11.2 mg). Method B: Rt: 0.97 min. m/z: 441.1 (M-H)” Exact mass: 442.0. 1H NMR (400 MHz, (0701) CHLOROFORM-d) delta ppm 1.39 (d, J=6.8 Hz, 3 H), 3.93 – 3.99 (m, 1 H), 4.00 (s, 3 H), 5.49 (d, J=46.9 Hz, 2 H), 7.37 (s, 1 H), 7.58 – 7.64 (m, 2 H), 8.52 (d, J=5.3 Hz, 1 H).

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 100114-58-7, 4-Amino-2-(hydroxymethyl)pyridine.

Reference:
Patent; JANSSEN SCIENCES IRELAND UC; VANDYCK, Koen; HACHE, Geerwin Yvonne Paul; LAST, Stefaan Julien; ROMBOUTS, Geert; VERSCHUEREN, Wim Gaston; RABOISSON, Pierre Jean-Marie Bernard; WO2015/118057; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 178876-83-0, 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. 178876-83-0, name is Methyl 6-amino-3-bromopicolinate, molecular formula is C7H7BrN2O2, 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.

a) 6-Amino-3-methyl-pyridine-2-carboxylic acid methyl ester; To a solution of 6-amino-3-bromo-pyridine-2-carboxylic acid methyl ester (3 g, 12.99 mmol) and trimethyl boroxine (1.8 mL, 2.99 mmol) in 1,4 dioxane (30 mL) was added K2CO3 (3.5 g, 25.97 mmol) under an argon atmosphere. To this was added PdCl2 (dppf)2.CH2Cl2 (530 mg, 0.65 mmol) and stirred at 115 C. for 4 h. The reaction mixture was cooled to room temperature and water was added to residue. The aqueous phase was extracted with ethyl acetate, the combined organic phases were dried over sodium sulfate, the solvent was evaporated and the residue purified by silica gel chromatography using ethyl acetate/hexane as eluent. The title compound was obtained as an off white solid (1.9 g, 88%).MS ESI (m/e): 166.8 [(M+H)+].1H NMR (DMSO, 400 MHz): delta(ppm)=7.31 (d, J=8.4 Hz, 1H), 6.53 (d, J=8.36 Hz, 1H), 5.99 (s, 2H), 3.77 (s, 3H), 2.21 (s, 3H).

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 178876-83-0, Methyl 6-amino-3-bromopicolinate.

Reference:
Patent; Baumann, Karlheinz; Goetschi, Erwin; Green, Luke; Jolidon, Synese; Knust, Henner; Limberg, Anja; Luebbers, Thomas; Thomas, Andrew; US2011/190269; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem