Extracurricular laboratory: Synthetic route of 3-Amino-5,6-dichloropyridine

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 98121-41-6, 3-Amino-5,6-dichloropyridine.

Electric Literature of 98121-41-6, 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 98121-41-6, name is 3-Amino-5,6-dichloropyridine. This compound has unique chemical properties. The synthetic route is as follows.

Example 2D 5-bromo-2,3-dichloropyridine A 5 L flask with mechanical stirrer, thermocouple, and addition funnel was charged with the product of Example 2C (70 g, 429 mmol) and 48% HBraq (240 mL). The suspension was maintained at 0-5 C. as a solution of NaNO2 (32.0 g, 464 mmol) in water (100 mL) was added dropwise over 1 hour. Additional water (200 mL) was added and the mixture was stirred for 10 minutes at 0-5 C. The mixture was treated with CuBr (32.6 g, 227 mmol) in portions over 20 minutes followed by additional water to maintain a fluid reaction mixture. The mixture was allowed to warm to room temperature and diluted with water. The mixture was distilled at ambient pressure, until the distillate ran clear (1.5 L collected). The distillate was extracted with EtOAc (3*500 mL) and the combined extracts were washed with brine (100 mL), dried (MgSO4), and concentrated to provide 5-bromo-2,3-dichloropyridine as a solid. 1H NMR (CDCl3, 300 MHz) delta 7.94 (d, J=3 Hz, 1H), 8.38 (d, J=3 Hz, 1H).

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 98121-41-6, 3-Amino-5,6-dichloropyridine.

Reference:
Patent; Buckley, Michael J.; Ji, Jianguo; US2005/261348; (2005); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Share a compound : 3-Amino-5,6-dichloropyridine

Statistics shows that 98121-41-6 is playing an increasingly important role. we look forward to future research findings about 3-Amino-5,6-dichloropyridine.

Electric Literature of 98121-41-6, 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.98121-41-6, name is 3-Amino-5,6-dichloropyridine, molecular formula is C5H4Cl2N2, molecular weight is 163.01, as common compound, the synthetic route is as follows.

Precursor alpha: 2,3-Dichloro-5-ethylthiopyridine 24.45 g (0.15 mol) of 3-amino-5,6-dichloropyridine in 280 ml of methylene chloride were reacted with 36.6 g (0.3 mol) of diethyl disulfide and 23.2 g (0.225 mol) of tert-butyl nitrite in 130 ml of methylene chloride by a method similar to Example 1, Precursor alpha. After working up and subsequently washing the crude product with ethanol, 13.3 g of product of value were obtained. Yield: 42%; 1H-NMR (in d6 dimethyl sulfoxide): delta [ppm]=1.25 (t, CH3); 3.10 (d, CH2); 8.15 and 8.3 (2*d, pyr H).

Statistics shows that 98121-41-6 is playing an increasingly important role. we look forward to future research findings about 3-Amino-5,6-dichloropyridine.

Reference:
Patent; BASF Aktiengesellschaft; US6448205; (2002); B1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

New learning discoveries about 98121-41-6

According to the analysis of related databases, 98121-41-6, the application of this compound in the production field has become more and more popular.

Synthetic Route of 98121-41-6, 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 98121-41-6, name is 3-Amino-5,6-dichloropyridine. This compound has unique chemical properties. The synthetic route is as follows.

A 5L flask with mechanical stirrer, thermocouple, and addition funnel was charged with the product of Example 2C (70 g, 429 mmol) and 48% HBraq (240 mL). The suspension was maintained at 0-5 C. as a solution of NaNO2 (32.0g, 464 mmol) in water (100 mL) was added dropwise over 1 hour. Additional water (200 mL) was added and the mixture was stirred for 10 minutes at 0-5 C. The mixture was treated with CuBr (32.6 g, 227 mmol) in portions over 20 minutes followed by additional water to maintain a fluid reaction mixture. The mixture was allowed to warm to room temperature and diluted with water. The mixture was distilled at ambient pressure, until the distillate ran clear (1.5 L collected). The distillate was extracted with EtOAc (3*500 mL) and the combined extracts were washed with brine (100 mL), dried (MgSO4), and concentrated to provide 5-bromo-2,3-dichloropyridine as a solid. 1H NMR (CDCl3, 300 MHz) delta 7.94 (d, J=3 Hz, 1H), 8.38 (d, J=3 Hz, 1H).

According to the analysis of related databases, 98121-41-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Buckley, Michael J.; Ji, Jianguo; US2004/242644; (2004); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

New learning discoveries about 98121-41-6

According to the analysis of related databases, 98121-41-6, the application of this compound in the production field has become more and more popular.

Synthetic Route of 98121-41-6, 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 98121-41-6, name is 3-Amino-5,6-dichloropyridine. This compound has unique chemical properties. The synthetic route is as follows.

A 5L flask with mechanical stirrer, thermocouple, and addition funnel was charged with the product of Example 2C (70 g, 429 mmol) and 48% HBraq (240 mL). The suspension was maintained at 0-5 C. as a solution of NaNO2 (32.0g, 464 mmol) in water (100 mL) was added dropwise over 1 hour. Additional water (200 mL) was added and the mixture was stirred for 10 minutes at 0-5 C. The mixture was treated with CuBr (32.6 g, 227 mmol) in portions over 20 minutes followed by additional water to maintain a fluid reaction mixture. The mixture was allowed to warm to room temperature and diluted with water. The mixture was distilled at ambient pressure, until the distillate ran clear (1.5 L collected). The distillate was extracted with EtOAc (3*500 mL) and the combined extracts were washed with brine (100 mL), dried (MgSO4), and concentrated to provide 5-bromo-2,3-dichloropyridine as a solid. 1H NMR (CDCl3, 300 MHz) delta 7.94 (d, J=3 Hz, 1H), 8.38 (d, J=3 Hz, 1H).

According to the analysis of related databases, 98121-41-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Buckley, Michael J.; Ji, Jianguo; US2004/242644; (2004); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Share a compound : 98121-41-6

The synthetic route of 98121-41-6 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 98121-41-6, 3-Amino-5,6-dichloropyridine, 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, Quality Control of 3-Amino-5,6-dichloropyridine, blongs to pyridine-derivatives compound. Quality Control of 3-Amino-5,6-dichloropyridine

Precursor alpha: 2,3-Dichloro-5-methylthiopyridine A solution of 50.6 g (0.3 mol) of 3-amino-5,6-dichloropyridine in 700 ml of methylene chloride was slowly added dropwise at 40 C. to a solution of 56.6 g (0.6 mol) of dimethyl disulfide and 46.7 g (0.45 mol) of tert-butyl nitrite in 320 ml of dry methylene chloride. The mixture was then stirred for 1 hour at 40 C. and subsequently for another approximately 15 hours at approximately 20 C., whereupon 500 ml of ice-water were added to the reaction mixture. The organic phase which was separated off was washed once with 1 N hydrochloric acid and once with water, dried over sodium sulfate and finally concentrated. After the crude product had been stirred with n-hexane, 21 g of a dark solid were obtained (purity 94% according to GC). After the hexane solution was concentrated, a further 21.3 g of product of value remained which had a purity of 77% (according to GC). Total yield: 62%; m.p.: 66-67 C.; 1H-NMR (in d6 dimethyl sulfoxide): delta [ppm]=2.6 (s, CH3); 8.1 and 8.3 (2*d, pyr H).

The synthetic route of 98121-41-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF Aktiengesellschaft; US6448205; (2002); B1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Analyzing the synthesis route of 98121-41-6

With the rapid development of chemical substances, we look forward to future research findings about 98121-41-6.

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. 98121-41-6, name is 3-Amino-5,6-dichloropyridine, molecular formula is C5H4Cl2N2, 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. Safety of 3-Amino-5,6-dichloropyridine

5-Amino-2,3-dichloropyridine (0.80 g) in dichloromethane (10 ml) was added to boron trifluoride etherate (0.92 ml) at -15 C. under nitrogen. Dichloromethane (15 ml) was added followed by t-butylnitrite (0.71 ml) in dichloromethane (5 ml). After 15 minutes the mixture was allowed to warm to -5 C. over 20 minutes. Hexane was added and the resulting solid was filtered, air-dried and washed with ether and stored at approximately -20 C. overnight. The solid was then heated until gas evolution had ceased and the product kugelrohr distilled to give 2,3-dichloro-5-fluoropyridine (0.104 g).

With the rapid development of chemical substances, we look forward to future research findings about 98121-41-6.

Reference:
Patent; Zeneca Limited; US5922732; (1999); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Analyzing the synthesis route of 98121-41-6

With the rapid development of chemical substances, we look forward to future research findings about 98121-41-6.

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. 98121-41-6, name is 3-Amino-5,6-dichloropyridine, molecular formula is C5H4Cl2N2, 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. Safety of 3-Amino-5,6-dichloropyridine

5-Amino-2,3-dichloropyridine (0.80 g) in dichloromethane (10 ml) was added to boron trifluoride etherate (0.92 ml) at -15 C. under nitrogen. Dichloromethane (15 ml) was added followed by t-butylnitrite (0.71 ml) in dichloromethane (5 ml). After 15 minutes the mixture was allowed to warm to -5 C. over 20 minutes. Hexane was added and the resulting solid was filtered, air-dried and washed with ether and stored at approximately -20 C. overnight. The solid was then heated until gas evolution had ceased and the product kugelrohr distilled to give 2,3-dichloro-5-fluoropyridine (0.104 g).

With the rapid development of chemical substances, we look forward to future research findings about 98121-41-6.

Reference:
Patent; Zeneca Limited; US5922732; (1999); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

The origin of a common compound about 3-Amino-5,6-dichloropyridine

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 98121-41-6, 3-Amino-5,6-dichloropyridine.

Electric Literature of 98121-41-6, 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. 98121-41-6, name is 3-Amino-5,6-dichloropyridine, molecular formula is C5H4Cl2N2, 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.

To a solution of 5,6-dichloro-pyridin-3-ylamine (40.0 g, 0.245 mol, 1.0 equiv.) in dichloromethane (300 mL) at 0 C was added boron trifluoride diethyl etherate (42.0 g, 0.296 mol, 1.2 equiv.) followed by 2-methyl-2-nitrosooxy-propane (38.0 g, 0.369 mol, 1.5 equiv.). The resulting reaction was allowed to warm to 25 C. The slurry of the product was stirred at this temperature for 30-60 min and filtered to afford 5,6-dichloro-pyridine-3-diazonium tetrafluoroborate (51.0 g, 0.195 mol).5,6-Dichloro-pyridine-3-diazonium tetrafluoroborate (180 g, 0.688 mol, 1.0 equiv.) was dissolved in Ac2O (540 mL) and stirred at RT for a few minutes. Then, the mixture was heated to 60 C. Acetic acid 5,6-dichloro-pyridin-3-yl ester was detected by LCMS. The acetic acid was evaporated, the precipitate was diluted with DCM and evaporated in vacuo. The mixture was purified on silica gel (1% EtOAc in petroleum ether as eluent) to afford acetic acid 5,6-dichloro-pyridin-3-yl ester (84.0 g, 0.408 mol).

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 98121-41-6, 3-Amino-5,6-dichloropyridine.

Reference:
Article; Duplessis, Martin; Morency, Louis; James, Clint; Minville, Joannie; Deroy, Patrick; Morin, Sebastien; Thavonekham, Bounkham; Tremblay, Martin; Halmos, Ted; Simoneau, Bruno; Bousquet, Yves; Sturino, Claudio; Tetrahedron Letters; vol. 54; 19; (2013); p. 2303 – 2307;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Introduction of a new synthetic route about 3-Amino-5,6-dichloropyridine

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,98121-41-6, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 98121-41-6, 3-Amino-5,6-dichloropyridine, 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, 98121-41-6, blongs to pyridine-derivatives compound. name: 3-Amino-5,6-dichloropyridine

EXAMPLE 11 5,6-dichloro-3-pyridinol Process (a) 8.15 g (50 mmol) of 3-amino-5,6-dichloropyridine were dissolved in 100 ml of 8N H2 SO4 and diazotized at 0 C. using 3.55 g (53 mmol) of sodium nitrite in 9 ml of water. The cold diazonium salt solution was added dropwise to 100 C. warm 60% strength sulfuric acid. After completion of the nitrogen elimination, the mixture was neutralized and extractively distilled using toluene. The dried toluene phase was concentrated by evaporation and the residue was recrystallized repeatedly from toluene. Melting point 184-185 C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,98121-41-6, its application will become more common.

Reference:
Patent; Hoechst Aktiengesellschaft; US4756739; (1988); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

A new synthetic route of 98121-41-6

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,98121-41-6, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 98121-41-6, 3-Amino-5,6-dichloropyridine, 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, 98121-41-6, blongs to pyridine-derivatives compound. name: 3-Amino-5,6-dichloropyridine

EXAMPLE 11 5,6-dichloro-3-pyridinol Process (a) 8.15 g (50 mmol) of 3-amino-5,6-dichloropyridine were dissolved in 100 ml of 8N H2 SO4 and diazotized at 0 C. using 3.55 g (53 mmol) of sodium nitrite in 9 ml of water. The cold diazonium salt solution was added dropwise to 100 C. warm 60% strength sulfuric acid. After completion of the nitrogen elimination, the mixture was neutralized and extractively distilled using toluene. The dried toluene phase was concentrated by evaporation and the residue was recrystallized repeatedly from toluene. Melting point 184-185 C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,98121-41-6, its application will become more common.

Reference:
Patent; Hoechst Aktiengesellschaft; US4756739; (1988); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem