Category: 5453-67-8

Synthetic Route of 5453-67-8, 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 5453-67-8 as follows.

Step 1: Preparation of methyl 6-formylpyridine-2-carboxylate (I-33a) A suspension of dimethylpyridine-2,6-dicarboxylate (1.0 g, 5.12 mmol) in methanol (8 mL) and THF (3 mL) was heated at 75 C. until the solid was dissolved. NaBH4 (184 mg, 4.87 mmol) was then added portion-wise. The mixture was stirred at 70 C. for 1 h. The mixture was cooled to room temperature and 10% citric acid (1.6 mL) was added. The solution was filtered and the filtrate was evaporated to dryness, taken up in dichloromethane, dried over MgSO4 and the solvent was removed in vacuo. The residue was purified by silica gel chromatography, eluting with 0-100% EtOAc in isohexane, to provide a colourless oil which was then dissolved in toluene (20 mL) and chloroform (20 mL). MnO2 (194 mg, 22.2 mmol) was added and the mixture was stirred at room temperature for 18 h. The mixture was filtered through a pad of fluorosil, eluting with chloroform (30 mL) and the solvent was removed in vacuo to provide the title compound (249 mg, 29%) as white solid. 1H NMR (400 MHz, CDCl3): delta 10.20 (s, 1H), 8.37 (dd, J=1.2, 7.6 Hz, 1H), 8.17 (dd, J=1.2, 7.6 Hz, 1H), 8.08-8.04 (m, 1H), 4.07 (s, 3H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,5453-67-8, its application will become more common.

Reference:
Patent; CHIESI FARMACEUTICI S.P.A.; AMARI, Gabriele; ARMANI, Elisabetta; GHIDINI, Eleonora; BAKER-GLENN, Charles; VAN DE POEL, Herve; WHITTAKER, Ben; US2015/158858; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 5453-67-8, 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.5453-67-8, name is Dimethyl pyridine-2,6-dicarboxylate, molecular formula is C9H9NO4, molecular weight is 195.17, as common compound, the synthetic route is as follows.

A suspension of dimethyl pyridine-2,6-dicarboxylate (1.0 g, 5.12 mmol) in methanol (8 mL) and THF (3 mL) was heated at 75C until the solid was dissolved.NaBH4 (184 mg, 4.87 mmol) was then added portion-wise. The mixture was stirred at70C for 1 h. The mixture was cooled to room temperature and 10% citric acid (1.6 mL)was added. The solution was filtered and the filtrate was evaporated to dryness, taken upin dichloromethane, dried over Mg504 and the solvent was removed in vacuo. Theresidue was purified by silica gel chromatography, eluting with 0-100% EtOAc in isohexane, to provide a colourless oil which was then dissolved in toluene (20 mL) and chloroform (20 mL). Mn02 (194 mg, 22.2 mmol) was added and the mixture was stirred at room temperature for 18 h. The mixture was filtered through a pad of fluorosil, eluting with chloroform (30 mL) and the solvent was removed in vacuo to provide the titlecompound (249 mg, 29%) as white solid.?H NMR (400 MHz, CDC13): oe 10.20 (s, 1 H), 8.37 (dd, J = 1.2, 7.6 Hz, 1 H), 8.17(dd, J = 1.2, 7.6 Hz, 1 H), 8.08-8.04 (m, 1 H), 4.07 (s, 3 H).

Statistics shows that 5453-67-8 is playing an increasingly important role. we look forward to future research findings about Dimethyl pyridine-2,6-dicarboxylate.

Reference:
Patent; CHIESI FARMACEUTICI S.P.A.; AMARI, Gabriele; ARMANI, Elisabetta; GHIDINI, Eleonora; BAKER-GLENN, Charles; VAN DE POeEL, Herve; WHITTAKER, Ben; WO2015/82616; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 5453-67-8, 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.5453-67-8, name is Dimethyl pyridine-2,6-dicarboxylate, molecular formula is C9H9NO4, molecular weight is 195.17, as common compound, the synthetic route is as follows.

A suspension of dimethyl pyridine-2,6-dicarboxylate (1.0 g, 5.12 mmol) in methanol (8 mL) and THF (3 mL) was heated at 75C until the solid was dissolved.NaBH4 (184 mg, 4.87 mmol) was then added portion-wise. The mixture was stirred at70C for 1 h. The mixture was cooled to room temperature and 10% citric acid (1.6 mL)was added. The solution was filtered and the filtrate was evaporated to dryness, taken upin dichloromethane, dried over Mg504 and the solvent was removed in vacuo. Theresidue was purified by silica gel chromatography, eluting with 0-100% EtOAc in isohexane, to provide a colourless oil which was then dissolved in toluene (20 mL) and chloroform (20 mL). Mn02 (194 mg, 22.2 mmol) was added and the mixture was stirred at room temperature for 18 h. The mixture was filtered through a pad of fluorosil, eluting with chloroform (30 mL) and the solvent was removed in vacuo to provide the titlecompound (249 mg, 29%) as white solid.?H NMR (400 MHz, CDC13): oe 10.20 (s, 1 H), 8.37 (dd, J = 1.2, 7.6 Hz, 1 H), 8.17(dd, J = 1.2, 7.6 Hz, 1 H), 8.08-8.04 (m, 1 H), 4.07 (s, 3 H).

Statistics shows that 5453-67-8 is playing an increasingly important role. we look forward to future research findings about Dimethyl pyridine-2,6-dicarboxylate.

Reference:
Patent; CHIESI FARMACEUTICI S.P.A.; AMARI, Gabriele; ARMANI, Elisabetta; GHIDINI, Eleonora; BAKER-GLENN, Charles; VAN DE POeEL, Herve; WHITTAKER, Ben; WO2015/82616; (2015); 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.5453-67-8, name is Dimethyl pyridine-2,6-dicarboxylate, molecular formula is C9H9NO4, molecular weight is 195.17, as common compound, the synthetic route is as follows.Application In Synthesis of Dimethyl pyridine-2,6-dicarboxylate

A solution of compound 6 (9.75 g, 50 mmol) in absolute ethanol (40 ml)and stirred in an ice bath as 7.8 g (4 eq.) of sodium borohydride wasadded in portion over 15 minutes, and the mixture was stirred at 0 for1 hour. The ice bath was removed and stirred at room temperature for 2hours, after which it was heated at reflux on a steam bath for 10 hours.The solvent was distilled in vacuo, the residue was mixed with 40 mL ofacetone, and heated on a steam bath for 1 h, and the solvent was distilledin vacuo. The residue was mixed with 40 mL of aqueous potassiumcarbonate and heated on a steam bath for 1 h, the solvent was distilledin vacuo, and the residue was dissolved in 100 mL of water. The aqueous solution was extracted continuously with CHCl3 for 10h to give 6 g (87%)of compound 7. 1H NMR (400 MHz, CDCl3) delta 7.70 (t, J = 7.6 Hz, 1H),7.20 (d, J = 7.7 Hz, 2H), 4.78 (s, 4H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5453-67-8, Dimethyl pyridine-2,6-dicarboxylate, and friends who are interested can also refer to it.

Reference:
Article; Yu, Kang-Kang; Li, Kun; Hou, Ji-Ting; Yu, Xiao-Qi; Tetrahedron Letters; vol. 54; 43; (2013); p. 5771 – 5774;,
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.5453-67-8, name is Dimethyl pyridine-2,6-dicarboxylate, molecular formula is C9H9NO4, molecular weight is 195.17, as common compound, the synthetic route is as follows.Application In Synthesis of Dimethyl pyridine-2,6-dicarboxylate

A solution of compound 6 (9.75 g, 50 mmol) in absolute ethanol (40 ml)and stirred in an ice bath as 7.8 g (4 eq.) of sodium borohydride wasadded in portion over 15 minutes, and the mixture was stirred at 0 for1 hour. The ice bath was removed and stirred at room temperature for 2hours, after which it was heated at reflux on a steam bath for 10 hours.The solvent was distilled in vacuo, the residue was mixed with 40 mL ofacetone, and heated on a steam bath for 1 h, and the solvent was distilledin vacuo. The residue was mixed with 40 mL of aqueous potassiumcarbonate and heated on a steam bath for 1 h, the solvent was distilledin vacuo, and the residue was dissolved in 100 mL of water. The aqueous solution was extracted continuously with CHCl3 for 10h to give 6 g (87%)of compound 7. 1H NMR (400 MHz, CDCl3) delta 7.70 (t, J = 7.6 Hz, 1H),7.20 (d, J = 7.7 Hz, 2H), 4.78 (s, 4H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5453-67-8, Dimethyl pyridine-2,6-dicarboxylate, and friends who are interested can also refer to it.

Reference:
Article; Yu, Kang-Kang; Li, Kun; Hou, Ji-Ting; Yu, Xiao-Qi; Tetrahedron Letters; vol. 54; 43; (2013); p. 5771 – 5774;,
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.5453-67-8, name is Dimethyl pyridine-2,6-dicarboxylate, molecular formula is C9H9NO4, molecular weight is 195.17, as common compound, the synthetic route is as follows.Application In Synthesis of Dimethyl pyridine-2,6-dicarboxylate

A solution of compound 6 (9.75 g, 50 mmol) in absolute ethanol (40 ml)and stirred in an ice bath as 7.8 g (4 eq.) of sodium borohydride wasadded in portion over 15 minutes, and the mixture was stirred at 0 for1 hour. The ice bath was removed and stirred at room temperature for 2hours, after which it was heated at reflux on a steam bath for 10 hours.The solvent was distilled in vacuo, the residue was mixed with 40 mL ofacetone, and heated on a steam bath for 1 h, and the solvent was distilledin vacuo. The residue was mixed with 40 mL of aqueous potassiumcarbonate and heated on a steam bath for 1 h, the solvent was distilledin vacuo, and the residue was dissolved in 100 mL of water. The aqueous solution was extracted continuously with CHCl3 for 10h to give 6 g (87%)of compound 7. 1H NMR (400 MHz, CDCl3) delta 7.70 (t, J = 7.6 Hz, 1H),7.20 (d, J = 7.7 Hz, 2H), 4.78 (s, 4H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,5453-67-8, Dimethyl pyridine-2,6-dicarboxylate, and friends who are interested can also refer to it.

Reference:
Article; Yu, Kang-Kang; Li, Kun; Hou, Ji-Ting; Yu, Xiao-Qi; Tetrahedron Letters; vol. 54; 43; (2013); p. 5771 – 5774;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 5453-67-8, 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. 5453-67-8, name is Dimethyl pyridine-2,6-dicarboxylate, molecular formula is C9H9NO4, 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.

Dimethyl pyridine-2,6-dicarboxylate (885g, leq) is dissolved in EtOH (4425g, 5 Volume) at room temperature. The NaBH4 (341 g, 2eq) is added slowly to the reaction while keeping the internal temperature below 30C using an ice bath. The reaction is heated to 35C forapproximately 2hrs. After reaction completion, the mixture is cooled to room temperature and adjusted with 32% HC1 solution to pH value of approximately 2.5. The mixture is stirred for 9 using 30% NaOH solution while maintaining an internal temperature below 30C and stirred at room temperature for about 30 mm. The solids are removed by filtration. The filtrate is concentrated at 50C. The concentrated residual is suspended with isopropanol (4160g, 8 vol)/water (416g, 0.8 vol) and heated to 70C for about lhr. The solution is then cooled to room temperature and stirred for 2hr before cooling to 5-10C for 30mm. The un-dissolved solids are removed by filtration. The filtrate is concentrated at 50C. The concentrated residue is charged with dichiommethane (2700g, Svol) and heated to 40 C for 30mm. The suspension is cooled to 5- 10C and stirred for 30mins. The solid is collected by filtration and dried under vacuum at 40C to obtain pyridine-2,6-diyldimethanol; 540.77g, purity 100%, yield 85.86%

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 5453-67-8, Dimethyl pyridine-2,6-dicarboxylate.

Reference:
Patent; CORVUS PHARMACEUTICALS, INC.; BY, Kolbot; JONES, William, Benton; WOLFE, Bradley, Hamilton; (131 pag.)WO2018/183965; (2018); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 5453-67-8, 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. 5453-67-8, name is Dimethyl pyridine-2,6-dicarboxylate, molecular formula is C9H9NO4, 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.

Dimethyl pyridine-2,6-dicarboxylate (885g, leq) is dissolved in EtOH (4425g, 5 Volume) at room temperature. The NaBH4 (341 g, 2eq) is added slowly to the reaction while keeping the internal temperature below 30C using an ice bath. The reaction is heated to 35C forapproximately 2hrs. After reaction completion, the mixture is cooled to room temperature and adjusted with 32% HC1 solution to pH value of approximately 2.5. The mixture is stirred for 9 using 30% NaOH solution while maintaining an internal temperature below 30C and stirred at room temperature for about 30 mm. The solids are removed by filtration. The filtrate is concentrated at 50C. The concentrated residual is suspended with isopropanol (4160g, 8 vol)/water (416g, 0.8 vol) and heated to 70C for about lhr. The solution is then cooled to room temperature and stirred for 2hr before cooling to 5-10C for 30mm. The un-dissolved solids are removed by filtration. The filtrate is concentrated at 50C. The concentrated residue is charged with dichiommethane (2700g, Svol) and heated to 40 C for 30mm. The suspension is cooled to 5- 10C and stirred for 30mins. The solid is collected by filtration and dried under vacuum at 40C to obtain pyridine-2,6-diyldimethanol; 540.77g, purity 100%, yield 85.86%

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 5453-67-8, Dimethyl pyridine-2,6-dicarboxylate.

Reference:
Patent; CORVUS PHARMACEUTICALS, INC.; BY, Kolbot; JONES, William, Benton; WOLFE, Bradley, Hamilton; (131 pag.)WO2018/183965; (2018); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem