Sep 2021 News Extracurricular laboratory: Synthetic route of 1121-76-2

Statistics shows that 1121-76-2 is playing an increasingly important role. we look forward to future research findings about 4-Chloropyridine 1-oxide.

Reference of 1121-76-2, 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.1121-76-2, name is 4-Chloropyridine 1-oxide, molecular formula is C5H4ClNO, molecular weight is 129.5444, as common compound, the synthetic route is as follows.

4-Chloro-2-(hydroxymethyl)pyridine : A solution of 4-CHLOROPYRIDINE ASOXIDE (5 G, 38.6 MMOL) and TRIMETHYLOXONIUM TETRAFLUOROBORATE (5.94 G, 40.1 MMOI) in CH2CL2 (115 mL) was stirred for two hours at ambient temperature. The solvent was evaporated and the residue taken up in MeOH (115 mL) and heated to near boiling. Ammonium persulfate (1.76 G, 7.72 MMOL) dissolved in H2O (7.7 mL) was added and the mixture was heated to reflux for 30 min. A second portion of ammonium persulfate (0.88 G) in H2O (3.9 mL) was added and the mixture was refluxed for another 30 min. The solvent was evaporated and the residue was partitioned between CHZCTZ and aqueous Na2CO3 (10% w/v). The organic layer was washed with H2O, dried over MgSO4 and evaporated leaving 2.4 G (43%) of the title compound. 1H NMR (CDC13) 8 8.20 (d, 1H, J=5. 0 Hz, H-6); 7.31 (s, 1H, H-3); 7.04 (d, 1H, J=5. 0 Hz, H-5); 5.46 (s, LH, OH); 4.61 (s, 2H, CH2).

Statistics shows that 1121-76-2 is playing an increasingly important role. we look forward to future research findings about 4-Chloropyridine 1-oxide.

Reference:
Patent; TRIGEN LIMITED; WO2005/12323; (2005); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Extended knowledge of 4-Chloropyridine 1-oxide

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, 1121-76-2, 4-Chloropyridine 1-oxide.

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. 1121-76-2, name is 4-Chloropyridine 1-oxide. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 4-Chloropyridine 1-oxide

4-Chloropyridine-N-oxide (3.0 g, 23 mmol), 4-trifluoromethylphenylboronic acid (6.57 g, 34.6 mmol), K2CO3 (4.8 g, 35 mmol) and PdCl2(dppf) (470 mg, 0.57 mmol) were stirred in DMSO (40 mL) under vacuum for 30 min. The flask was flushed with nitrogen, and the mixture was heated to 80 C. for 10 min. Upon cooling, the mixture was diluted with methylene chloride and washed with 5% lithium chloride solution (5*), dried, concentrated, and the residue was purified by flash column chromatography (40 g ISCO column eluting with methylene chloride and a methanol/ammonia mixture (10:1); gradient 100% methylene chloride to 80% methylene chloride over 30 min at 40 mL/min) to provide the title compound (1.90 g, 34%) as a tan solid: ESI MS m/z 240 [M+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, 1121-76-2, 4-Chloropyridine 1-oxide.

Reference:
Patent; ALBANY MOLECULAR RESEARCH, INC.; US2012/157460; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Introduction of a new synthetic route about 1121-76-2

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1121-76-2, 4-Chloropyridine 1-oxide, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 1121-76-2, 4-Chloropyridine 1-oxide, 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, category: pyridine-derivatives, blongs to pyridine-derivatives compound. category: pyridine-derivatives

4-(4-Chloro-benzyloxy)-py?dine-N-oxide: To a suspension of powdered potassium hydroxide (7.60 g, 136 mmol) and potassium carbonate (4.70 g, 34.1 mmol) in dry toluene were added (4-chloro-phenyl)-methanol (7.26 g, 50.9 mmol), 4-chloropyridinc-N-oxide (4.39 g, 34.0 mmol) and TDA-I (1.10 mL, 3.44 mmol). After the mixture was heated at reflux for 3 hours, the organic layer was separated and dried over anhydrous sodium sulfate. The solvent was removed in vacuo and the residue was purified through a silica gel column to give 4-(4-chloro-benzyloxy)-pyridine-N-oxide in 40% yield as light yellowish solid. 1H NMR (CDCl1) 5: 8.13 (m, 2H), 7.37 (m, 4H), 6.85 (m, 2H), 5.06 (s, 2H); ESMS m/e: 235.9 (M+H)+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1121-76-2, 4-Chloropyridine 1-oxide, and friends who are interested can also refer to it.

Reference:
Patent; H. LUNDBECK A/S; WO2009/120655; (2009); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Analyzing the synthesis route of 1121-76-2

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 1121-76-2, 4-Chloropyridine 1-oxide.

Reference of 1121-76-2, 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 1121-76-2, name is 4-Chloropyridine 1-oxide. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A solution of (4-chloropheny)methanol (49.5 g, 347 mmol) inTHF (200 mL) was added dropwise to a suspension of NaH (60%oil dispersion, 16.7 g, 419 mmol) in THF (200 mL) at 0 C. Afterthe mixture was stirred at 0 C for 30 min, 4 (45.0 g, 347 mmol)was added portionwise to the reaction mixture. After completionof the addition, the mixture was stirred at rt for 5 h. The mixturewas quenched with water (400 mL) at 0 C and extracted withEtOAc/THF (1:1) four times. The organic layers were combined,passed through NH-silica gel pad (EtOAc/MeOH) and concentrated.The filtrate was concentrated, and the residual solid was washedwith IPE and dried to give the title compound (54.3 g, 66%) as abrown solid.

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 1121-76-2, 4-Chloropyridine 1-oxide.

Reference:
Article; Igawa, Hideyuki; Takahashi, Masashi; Ikoma, Minoru; Kaku, Hiromi; Kakegawa, Keiko; Kina, Asato; Aida, Jumpei; Okuda, Shoki; Kawata, Yayoi; Noguchi, Toshihiro; Hotta, Natsu; Yamamoto, Syunsuke; Nakayama, Masaharu; Nagisa, Yasutaka; Kasai, Shizuo; Maekawa, Tsuyoshi; Bioorganic and Medicinal Chemistry; vol. 24; 11; (2016); p. 2504 – 2518;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

New learning discoveries about 1121-76-2

The synthetic route of 1121-76-2 has been constantly updated, and we look forward to future research findings.

Reference of 1121-76-2 , The common heterocyclic compound, 1121-76-2, name is 4-Chloropyridine 1-oxide, molecular formula is C5H4ClNO, 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.

A mixture of 4-chloropyridine, 1 -oxide (0.0025 mol), Pd2(dba)3 (catalytic quantity), Xantphos (catalytic quantity) and Cs2CO3 (0.973 g) in dioxane (5ml) was degassed by applying alternating N2 atmosphere and vacuum. Intermediate (70) (0.0023 mol) in dioxane (15ml) was added under N2-atmosphere. The reaction mixture was stirred at 1000C for 2 hours. The mixture was extracted (DCM/H2O), dried, filtered and evaporated. The residue was used crude, yielding intermediate (71).

The synthetic route of 1121-76-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; WO2008/3665; (2008); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Brief introduction of 1121-76-2

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1121-76-2, 4-Chloropyridine 1-oxide, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 1121-76-2, 4-Chloropyridine 1-oxide, 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: C5H4ClNO, blongs to pyridine-derivatives compound. COA of Formula: C5H4ClNO

Reference Example 110 4-Chloro-2-cyanopyridine 4-Chloropyridine N-oxide (7.53 g, 58.1 mmol) and N,N-dimethylcarbamoyl chloride (9.36 g, 87.0 mmol) were added to acetonitrile (200 ml), and trimethylsilyl cyanide (11.5 g, 116 mmol) was added dropwise thereto.. The mixture was stirred at room temperature for 18 hrs.. The reaction mixture was combined with ethyl acetate and water.. The organic layer was successively washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine and dried over magnesium sulfate.. The solvent was evaporated, and the residue was subjected to a silica gel (200 g) column chromatography.. The fractions eluted with n-hexane-ethyl acetate (3:1, v/v) were collected, concentrated to give the titled compound (8.05 g, 99 %) as a pale yellow oil.1H-NMR (CDCl3) delta: 7.54-7.56 (1H, m), 7.72(1H, s), 8.63 (1H, d, J = 5.3 Hz). IR(KBr): 2239, 1568, 1549, 1462, 1379, 1288, 1215, 844, 704 cm-1.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1121-76-2, 4-Chloropyridine 1-oxide, and friends who are interested can also refer to it.

Reference:
Patent; Takeda Chemical Industries, Ltd.; EP1424336; (2004); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

New learning discoveries about 1121-76-2

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 1121-76-2, 4-Chloropyridine 1-oxide.

Synthetic Route of 1121-76-2, 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. 1121-76-2, name is 4-Chloropyridine 1-oxide, molecular formula is C5H4ClNO, 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-Chloropyridine-N-oxide (3.0 g, 23 mmol), 4-trifluoromethylphenylboronic acid (6.57 g, 34.6 mmol), K2CO3 (4.8 g, 35 mmol) and PdCl2(dppf) (470 mg, 0.57 mmol) were stirred in DMSO (40 mL) under vacuum for 30 min. The flask was flushed with nitrogen, and the mixture was heated to 80 C. for 10 min. Upon cooling, the mixture was diluted with methylene chloride and washed with 5% lithium chloride solution (5×), dried, concentrated, and the residue was purified by flash column chromatography (40 g ISCO column eluting with methylene chloride and a methanol/ammonia mixture (10:1); gradient 100% methylene chloride to 80% methylene chloride over 30 min at 40 mL/min) to provide the title compound (1.90 g, 34%) as a tan solid: ESI MS m/z 240 [M+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 1121-76-2, 4-Chloropyridine 1-oxide.

Reference:
Patent; ALBANY MOLECULAR RESEARCH, INC.; US2011/3793; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

The origin of a common compound about 4-Chloropyridine 1-oxide

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1121-76-2, 4-Chloropyridine 1-oxide, and friends who are interested can also refer to it.

Synthetic Route of 1121-76-2, 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. 1121-76-2, name is 4-Chloropyridine 1-oxide. A new synthetic method of this compound is introduced below.

4-Chloropyridine-N-oxide (3.0 g, 23 mmol), 4-trifluoromethylphenylboronic acid (6.57 g, 34.6 mmol), K2CO3 (4.8 g, 35 mmol) and PdCl2 (dppf) (470 mg, 0.57 mmol) were stirred in DMSO (40 mL) under vacuum for 30 min. The flask was flushed with nitrogen, and the mixture was heated to 80 C. for 10 min. Upon cooling, the mixture was diluted with methylene chloride and washed with 5% lithium chloride solution (5¡Á), dried, concentrated, and the residue was purified by flash column chromatography (40 g ISCO column eluting with methylene chloride and a methanol/ammonia mixture (10:1); gradient 100% methylene chloride to 80% methylene chloride over 30 min at 40 mL/min) to provide the title compound (1.90 g, 34%) as a tan solid: ESI MS m/z 240 [M+H]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1121-76-2, 4-Chloropyridine 1-oxide, and friends who are interested can also refer to it.

Reference:
Patent; ALBANY MOLECULAR RESEARCH, INC.; US2011/3738; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem