Category: 88912-24-7

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.88912-24-7, name is 5,6-Dichloropicolinic acid, molecular formula is C6H3Cl2NO2, molecular weight is 192, as common compound, the synthetic route is as follows.COA of Formula: C6H3Cl2NO2

Sodium hydride (CAN 7646-69-7, 60% w/w, 1.05 g, 26 mmol) was added to cyclopropylmethanol (CAN 2516-33-8, 7.5 g) at 0 C. and the mixture was stirred for 1 h. 5,6-Dichloro-pyridine-2-carboxylic acid (1 g, 5 mmol) was added and the mixture was heated to 95 C. for 3 h. The solvent was removed under reduced pressure. The residue was diluted with water (10 mL) and adjusted to pH=3.0 by hydrochloric acid (3 N). The solution was extracted with ethyl acetate (3×15 mL). The combined organic layers were washed with water (3×30 mL) and brine (2×40 mL) and evaporated to dryness to give the crude product (0.35 g, 25%), which was used in the next step without further purification, MS (EI): m/e=228.1 [M+H]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,88912-24-7, 5,6-Dichloropicolinic acid, and friends who are interested can also refer to it.

Reference:
Patent; Bissantz, Caterina; Grether, Uwe; Hebeisen, Paul; Kimbara, Atsushi; Liu, Qingping; Nettekoven, Matthias; Prunotto, Marco; Roever, Stephan; Rogers-Evans, Mark; Schulz-Gasch, Tanja; Ullmer, Christoph; Wang, Zhiwei; Yang, Wulun; US2012/316147; (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.88912-24-7, name is 5,6-Dichloropicolinic acid, molecular formula is C6H3Cl2NO2, molecular weight is 192, as common compound, the synthetic route is as follows.COA of Formula: C6H3Cl2NO2

Sodium hydride (CAN 7646-69-7, 60% w/w, 1.05 g, 26 mmol) was added to cyclopropylmethanol (CAN 2516-33-8, 7.5 g) at 0 C. and the mixture was stirred for 1 h. 5,6-Dichloro-pyridine-2-carboxylic acid (1 g, 5 mmol) was added and the mixture was heated to 95 C. for 3 h. The solvent was removed under reduced pressure. The residue was diluted with water (10 mL) and adjusted to pH=3.0 by hydrochloric acid (3 N). The solution was extracted with ethyl acetate (3×15 mL). The combined organic layers were washed with water (3×30 mL) and brine (2×40 mL) and evaporated to dryness to give the crude product (0.35 g, 25%), which was used in the next step without further purification, MS (EI): m/e=228.1 [M+H]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,88912-24-7, 5,6-Dichloropicolinic acid, and friends who are interested can also refer to it.

Reference:
Patent; Bissantz, Caterina; Grether, Uwe; Hebeisen, Paul; Kimbara, Atsushi; Liu, Qingping; Nettekoven, Matthias; Prunotto, Marco; Roever, Stephan; Rogers-Evans, Mark; Schulz-Gasch, Tanja; Ullmer, Christoph; Wang, Zhiwei; Yang, Wulun; US2012/316147; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 88912-24-7, 5,6-Dichloropicolinic 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, Recommanded Product: 5,6-Dichloropicolinic acid, blongs to pyridine-derivatives compound. Recommanded Product: 5,6-Dichloropicolinic acid

To a 100 ml round bottom flask equipped with a magnetic stirrer, reflux condenser and a nitrogen inlet were added 5,6-dichioropicolinic acid (5.00 g, 23.1 mmol), TEA (8.3 g, 81.0 mmol), ACN (39.9 g) and water (15.3 g). The solution was sparged for 30 mm with nitrogen (1 mE/mm) After sparging, 1,1 ?-bis(diphenylphosphino)ferrocene (dppf; 0.19 g, 0.343 mmol) and palladium(II) acetate (0.08 g, 0.356 mmol) were added to the solution. (4-Chioro-2-fluoro-3- methoxyphenyl)boronic acid 5.4 g, 26.9 mmol) was added in one portion, and heating was initiated. The reaction mixture was heated to 550 C., and was sampled and analyzed periodically by liquid chromatography. No boronic acid was remaining after 22 hours, and heating was stopped. The reaction mixture was allowed to cool to 45 C. Once at temperature, 50% sulfuric acid (7.2 g) was added. No precipitation was observed, so the mixture was cooled. A precipitate formed, which was isolated by filtration. The flask was rinsed with cold mother liquor to isolate all of the product. The wetcake was then rinsed with cold ACN- water solution (8.75 g and 11.25 g, respectively). The palladium content was analyzed in the wetcake, wash and mother liquors, with 96% of the palladium in the mother liquor and wash, and 4% in the wet cake. 98% of the total palladium added was recovered.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,88912-24-7, 5,6-Dichloropicolinic acid, and friends who are interested can also refer to it.

Reference:
Patent; Dow AgroSciences LLC; Biswas, Sanjib; Chakrabarti, Reetam; Huffman, Lauren M.; Leng, Ronald B.; Schuitman, Abraham D.; Spiers, Karin; Stottlemyer, Alan L.; Epp, Jeffrey B.; (18 pag.)US2016/340311; (2016); A1;,
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. 88912-24-7, name is 5,6-Dichloropicolinic acid, the common compound, a new synthetic route is introduced below. Safety of 5,6-Dichloropicolinic acid

EXAMPLE 14 5,6-bis(ethylthio)-2-pyridinecarboxylic acid Potassium t-butoxide (111 g) was stirred in 200 ml of DMSO under N2. The reaction vessel was cooled with an ice bath while ethanethiol (43 g) was added, and the mixture was stirred for 30 minutes. The cold bath was removed, and 5,6-dichloro-2-pyridinecarboxylic acid (55 g) in 300 ml of DMSO was added. The mixture was stirred at 75 C. for 20 hours. After cooling, the mixture was added to 2 liters of ice water, then acidified with concentrated HCl. The white solid which formed was collected and dried to give 66.15 g of the crude product. A portion of the crude product was recrystallized from isopropanol which gave purified 5,6-bis(ethylthio)-2-pyridinecarboxylic acid, m.p. 112-113 C. Other bis(R-thio)pyridines were prepared by the decarboxylation of the appropriate bis(R-thio)-2-pyridinecarboxylic acid using the procedures described herein. These compounds are:

The synthetic route of 88912-24-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The Dow Chemical Company; US4616087; (1986); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 88912-24-7, 5,6-Dichloropicolinic 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, Recommanded Product: 5,6-Dichloropicolinic acid, blongs to pyridine-derivatives compound. Recommanded Product: 5,6-Dichloropicolinic acid

To a 100 ml round bottom flask equipped with a magnetic stirrer, reflux condenser and a nitrogen inlet were added 5,6-dichioropicolinic acid (5.00 g, 23.1 mmol), TEA (8.3 g, 81.0 mmol), ACN (39.9 g) and water (15.3 g). The solution was sparged for 30 mm with nitrogen (1 mE/mm) After sparging, 1,1 ?-bis(diphenylphosphino)ferrocene (dppf; 0.19 g, 0.343 mmol) and palladium(II) acetate (0.08 g, 0.356 mmol) were added to the solution. (4-Chioro-2-fluoro-3- methoxyphenyl)boronic acid 5.4 g, 26.9 mmol) was added in one portion, and heating was initiated. The reaction mixture was heated to 550 C., and was sampled and analyzed periodically by liquid chromatography. No boronic acid was remaining after 22 hours, and heating was stopped. The reaction mixture was allowed to cool to 45 C. Once at temperature, 50% sulfuric acid (7.2 g) was added. No precipitation was observed, so the mixture was cooled. A precipitate formed, which was isolated by filtration. The flask was rinsed with cold mother liquor to isolate all of the product. The wetcake was then rinsed with cold ACN- water solution (8.75 g and 11.25 g, respectively). The palladium content was analyzed in the wetcake, wash and mother liquors, with 96% of the palladium in the mother liquor and wash, and 4% in the wet cake. 98% of the total palladium added was recovered.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,88912-24-7, 5,6-Dichloropicolinic acid, and friends who are interested can also refer to it.

Reference:
Patent; Dow AgroSciences LLC; Biswas, Sanjib; Chakrabarti, Reetam; Huffman, Lauren M.; Leng, Ronald B.; Schuitman, Abraham D.; Spiers, Karin; Stottlemyer, Alan L.; Epp, Jeffrey B.; (18 pag.)US2016/340311; (2016); A1;,
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. 88912-24-7, name is 5,6-Dichloropicolinic acid, the common compound, a new synthetic route is introduced below. Safety of 5,6-Dichloropicolinic acid

EXAMPLE 14 5,6-bis(ethylthio)-2-pyridinecarboxylic acid Potassium t-butoxide (111 g) was stirred in 200 ml of DMSO under N2. The reaction vessel was cooled with an ice bath while ethanethiol (43 g) was added, and the mixture was stirred for 30 minutes. The cold bath was removed, and 5,6-dichloro-2-pyridinecarboxylic acid (55 g) in 300 ml of DMSO was added. The mixture was stirred at 75 C. for 20 hours. After cooling, the mixture was added to 2 liters of ice water, then acidified with concentrated HCl. The white solid which formed was collected and dried to give 66.15 g of the crude product. A portion of the crude product was recrystallized from isopropanol which gave purified 5,6-bis(ethylthio)-2-pyridinecarboxylic acid, m.p. 112-113 C. Other bis(R-thio)pyridines were prepared by the decarboxylation of the appropriate bis(R-thio)-2-pyridinecarboxylic acid using the procedures described herein. These compounds are:

The synthetic route of 88912-24-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The Dow Chemical Company; US4616087; (1986); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 88912-24-7, 5,6-Dichloropicolinic 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, 88912-24-7, blongs to pyridine-derivatives compound. Recommanded Product: 88912-24-7

Sodium hydride (CAN 7646-69-7, 60% w/w, 1.05 g, 26 mmol) was added tocyclopropylmethanol (CAN 2516-33-8, 7.5 g) at 0C and the mixture was stirred for 1 h. 5,6-Dichloro-pyridine-2-carboxylic acid (1 g, 5 mmol) was added and the mixture was heated to 95C for 3 h. The solvent was removed under reduced pressure. The residue was diluted with water (10 mL) and adjusted to pH = 3.0 by hydrochloric acid (3 N). The solution was extracted with ethyl acetate (3 x 15 mL). The combined organic layers were washed with water (3 x 30 mL) and brine (2 x 40 mL) and evaporated to dryness to give the crude product (0.35 g, 25%>), which was used in the next step without further purification, MS (EI): m/e = 228.1 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,88912-24-7, its application will become more common.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; BISSANTZ, Caterina; GRETHER, Uwe; HEBEISEN, Paul; KIMBARA, Atsushi; LIU, Qingping; NETTEKOVEN, Matthias; PRUNOTTO, Marco; ROEVER, Stephan; ROGERS-EVANS, Mark; SCHULZ-GASCH, Tanja; ULLMER, Christoph; WANG, Zhiwei; YANG, Wulun; WO2012/168350; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 88912-24-7 ,Some common heterocyclic compound, 88912-24-7, molecular formula is C6H3Cl2NO2, 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.

EXAMPLE 12 2,3-bis(methylthio)pyridine In a 4-necked flask equipped with a Dry Ice condenser, mechanical stirrer, thermometer and dropping funnel, 172.2 g of t-BuOK was dissolved in 200 ml of DMSO at room temperature with stirring under N2. The solution was cooled with an ice bath while 50.0 g of methanethiol was added. The mixture was stirred for 30 minutes, then the ice bath was removed. A solution of 5,6-dichloro-2-pyridinecarboxylic acid (90.6 g) in 250 ml of DMSO was added at a rate such that the exotherm did not cause the temperature of the mixture to exceed 75 C. A dense slurry formed. An additional 500 ml of DMSO was added, and the slurry was stirred for 42 hours at 60 C. After cooling to room temperature, 500 ml of water was added to the reaction mixture, which was then added to 3.5 liters of ice water, and acidified to pH 1 with concentrated HCl. The yellow precipitate which formed was collected and dried which gave 87.33 g of a mixture of 5-chloro-6-(methylthio)-2-pyridinecarboxylic acid (~3.36 g) and 5,6-bis(methylthio)-2-pyridinecarboxylic acid (~83.97 g). The relative amounts of the 5-chloro-6-(methylthio)-2-pyridinecarboxylic acid and 5,6-bis(methylthio)-2-pyridinecarboxylic acid were estimated based on the amounts of the mono and bis-adducts isolated after decarboxylation.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,88912-24-7, its application will become more common.

Reference:
Patent; The Dow Chemical Company; US4616087; (1986); 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 88912-24-7, name is 5,6-Dichloropicolinic acid. This compound has unique chemical properties. The synthetic route is as follows. category: pyridine-derivatives

To a 100 mE round bottom flask equipped with a magnetic stirrer, reflux condenser and a nitrogen inlet were added 5,6-dichioropicolinic acid (5.00 g, 23.1 mmol), TEA (8.2 g, 81.0 mmol), ACN (39.5 g) and water (15.1 g). The solution was sparged for 30 mm with nitrogen (1 mE/mm) Afier sparging, triphenylphosphine (TPP; 0.18 g, 0.686 mmol) and palladium(II) acetate (0.078 g, 0.347 mmol) were added to the solution. Furan-2-boronic acid (3.3 g, 28.9 mmol) was added in one portion, and heating was initiated. The reaction mixture was heated to 55 C., and was sampled and analyzed by liquid chromatography. No boronic acid was remaining after two hours, and heating was stopped. The reaction mixture was allowed to cool overnight and then was heated to 45 C. Once at temperature, 50% sulfuric acid (7.1 g) was added. No precipitation was observed, so the mixture was cooled. After 30 mm at <5 C., no solids were observed and water (25.7 g) was added. A precipitate formed which was allowed to cool for 1 h and isolated by filtration. The flask was rinsed with cold mother liquor to isolate all of the product. The wetcake was then rinsed with cold ACN- water solution (8.75 g and 11.25 g, respectively). The palladium content was analyzed in the wetcake, wash and mother liquors, with 81% of the palladium in the mother liquor and wash, and 19% in the wet cake. 99% of the total palladium added was recovered. With the rapid development of chemical substances, we look forward to future research findings about 88912-24-7. Reference:
Patent; Dow AgroSciences LLC; Biswas, Sanjib; Chakrabarti, Reetam; Huffman, Lauren M.; Leng, Ronald B.; Schuitman, Abraham D.; Spiers, Karin; Stottlemyer, Alan L.; Epp, Jeffrey B.; (18 pag.)US2016/340311; (2016); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 88912-24-7, 5,6-Dichloropicolinic 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, Safety of 5,6-Dichloropicolinic acid, blongs to pyridine-derivatives compound. Safety of 5,6-Dichloropicolinic acid

A four-neck 500 milliliter (mL) round bottomed flask was fitted with a thermocouple/J-KEM controller, mechanical stirrer, condenser that vented to a knock-out pot then to a 12% sodium hydroxide (NaOH) scrubber and a stopper. To the vessel was added concentrated sulfuric acid (H2SO4; 27.0 grams (g), 0.28 moles (mol)) and sulfolane (28.9 g). This mixture was warmed to 130 C. and then the solid trichloromethyl-pyridine (70.2 g, 0.26 mol) was added in portions over ca. 1 hour (h). Vigorous degassing to the caustic trap was observed. After the addition was complete, the mixture was stirred at 130 C. for 2 h and then allowed to cool to room temperature with stirring overnight resulting in a thick taffy. The mixture was warmed to 70 C., and a sample was taken for high performance liquid chromatography (HPLC) analysis which indicated a very clean conversion to the corresponding carboxylic acid. To the pot at 70 C. was carefully added isopropyl alcohol (IPA; 83.2 g, 1.39 mol) in portions over about 45 minutes (min) Initially there was vigorous degassing to the NaOH/caustic trap. After the addition was complete, the clear brown solution was stirred at 70 C. for 1 h. The 70 C. solution was added to crushed ice (361 g) with swirling of the flask. At the end of the addition, there was very little ice in the slurry. The slurry was cooled in the refrigerator for 1 h, and the solid was collected via filtration. The cake was washed with IPA/water (31 g/31 g) and then water (65 g). The material was allowed to air dry in a hood to a constant weight providing the product as a light beige solid (55 g, ca. 89%): HPLC purity was 98.5%; EIMS (70 eV) m/z 235, 233 (M+, 1%, 2%), 220, 218, 194, 192, 176, 174, 149, 147 (100%); 1H NMR (400 MHz, CDCl3) 7.98, 7.91 (ABq, J=8.0 Hz, 2H), 5.30 (m, 1H), 1.41 (d, J=4.0 Hz, 6H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,88912-24-7, 5,6-Dichloropicolinic acid, and friends who are interested can also refer to it.

Reference:
Patent; Allen, Laura; Sanford, Melanie; Lee, Shin Hee; Bland, Douglas; Cheng, Yang; Roth, Gary; Muhuhi, Joseck M.; US2015/141654; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem