Category: 695-98-7

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.695-98-7, name is 2,3,5-Trimethylpyridine, molecular formula is C8H11N, molecular weight is 121.1796, as common compound, the synthetic route is as follows.SDS of cas: 695-98-7

In dichloromethane (15.0 ml), 2,3,5-trimethyl-pyridine (manufactured by Tokyo Kasei Kogyo Co., Ltd.) (1.29 g) was dissolved. After having been cooled to 0 C, the reaction solution was added with m-chloroperbenzoic acid (2.53 g), followed by stirring at room temperature for 1.5 hours. The reaction solution was added with a 1 mol/l sodium hydroxide aqueous solution and then subjected to extraction with chloroform. Subsequently, the organic layer was washed with a saturated saline solution and dried with anhydrous sodium sulfate. The drying agent was filtrated out and the solvent was then distilled off, followed by dissolving the resultant residue in dichloromethane (25.0 ml) . The reaction solution was added with trifluoroacetic anhydride (2.8 ml) and the whole was refluxed under heating for 3.5 hours. After the reaction solution was cooled to room temperature, the solvent was distilled off. The resultant residue was dissolved in methanol (60.0 ml). After having been cooled to 0C, the reaction solution was added with a 12.5% sodiummethoxide/methanol solution to adj ust the solution to pH 10, and the whole was stirred at room temperature for 16.5 hours. After the solvent was distilled off, the residue was added with distilled water and subjected to extraction with chloroform. The organic layer was washed with a saturated saline solution and dried with anhydrous sodium sulfate. The drying agent was filtrated out and the solvent was then distilled off, followed by dissolving the residue in chloroform (30.0 ml). The reaction solution was added with manganese dioxide (chemically processed product) (6.10 g) and then stirred at room temperature for 18 hours. The reaction solution was filtrated through Celite. The solvent in the filtrate was distilled off and the resultant residue was then purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (1.14 g) as a yellow oily substance. MS(FAB,Pos.):m/z=136[M+H]+ 1H-NMR(500MHz,CDCl3):delta=2.40(3H,s), 2.63(3H,s), 7.43(1H,brs), 8.48(1H,brs),10.16(1H,s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,695-98-7, 2,3,5-Trimethylpyridine, and friends who are interested can also refer to it.

Reference:
Patent; Kureha Corporation; EP1724263; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 695-98-7, 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 695-98-7 as follows.

In dichloromethane (15.0 ml), 2,3,5-trimethyl-pyridine (1.29 g) was dissolved. The reaction solution was cooled to 0°C and added with meta-chloroperbenzoic acid (2.53 g), followed by stirring at room temperature for 1.5 hours. The reaction solution was added with a 1 mol/l sodium hydroxide aqueous solution and then subjected to extraction with chloroform. Subsequently, the organic layer was washed with saturated saline solution and dried with anhydrous sodium sulfate. The drying agent was filtrated out and the solvent was then distilled off, followed by dissolving the resulting residue in dichloromethane (25.0 ml). The reaction solution was added with trifluoroacetic anhydride (2.8 ml) and subjected to thermal reflux for 3.5 hours. After the reaction solution had been cooled to room temperature, the solvent was distilled off. The residue obtained was dissolved in methanol (60.0 ml). After having been cooled to 0°C, the reaction solution was added with a 12.5percent sodium methoxide/methanol solution to adjust to pH 10, followed by stirring at room temperature for 16.5 hours. After the solvent had been distilled off, the residue was added with distilled water and extracted with chloroform. The organic layer was washed with saturated saline solution and dried with anhydrous sodium sulfate. The drying agent was filtrated out and the solvent was then distilled off, followed by dissolving the resulting residue in chloroform (30.0 ml). The reaction solution was added with manganese dioxide (chemically processed product) (6.10 g) and then stirred at room temperature for 18 hours. The reaction solution was filtrated through Celite. The solvent in the filtrate was distilled off and the residue obtained was then purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (1.14 g) as a yellow oily substance. MS(FAB,Pos.):m/z=136[M+H]+1H-NMR(500MHz,CDCl3):delta=2.40(3H,s),2.63(3H,s),7.43(1H,brs),8.48(1 H,brs),10.16(1H,s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,695-98-7, its application will become more common.

Reference:
Patent; Kureha Chemical Industry Co., Ltd.; EP1550657; (2005); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 695-98-7, 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 695-98-7 as follows.

In dichloromethane (15.0 ml), 2,3,5-trimethyl-pyridine (1.29 g) was dissolved. The reaction solution was cooled to 0°C and added with meta-chloroperbenzoic acid (2.53 g), followed by stirring at room temperature for 1.5 hours. The reaction solution was added with a 1 mol/l sodium hydroxide aqueous solution and then subjected to extraction with chloroform. Subsequently, the organic layer was washed with saturated saline solution and dried with anhydrous sodium sulfate. The drying agent was filtrated out and the solvent was then distilled off, followed by dissolving the resulting residue in dichloromethane (25.0 ml). The reaction solution was added with trifluoroacetic anhydride (2.8 ml) and subjected to thermal reflux for 3.5 hours. After the reaction solution had been cooled to room temperature, the solvent was distilled off. The residue obtained was dissolved in methanol (60.0 ml). After having been cooled to 0°C, the reaction solution was added with a 12.5percent sodium methoxide/methanol solution to adjust to pH 10, followed by stirring at room temperature for 16.5 hours. After the solvent had been distilled off, the residue was added with distilled water and extracted with chloroform. The organic layer was washed with saturated saline solution and dried with anhydrous sodium sulfate. The drying agent was filtrated out and the solvent was then distilled off, followed by dissolving the resulting residue in chloroform (30.0 ml). The reaction solution was added with manganese dioxide (chemically processed product) (6.10 g) and then stirred at room temperature for 18 hours. The reaction solution was filtrated through Celite. The solvent in the filtrate was distilled off and the residue obtained was then purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (1.14 g) as a yellow oily substance. MS(FAB,Pos.):m/z=136[M+H]+1H-NMR(500MHz,CDCl3):delta=2.40(3H,s),2.63(3H,s),7.43(1H,brs),8.48(1 H,brs),10.16(1H,s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,695-98-7, its application will become more common.

Reference:
Patent; Kureha Chemical Industry Co., Ltd.; EP1550657; (2005); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 695-98-7, 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. 695-98-7, name is 2,3,5-Trimethylpyridine, molecular formula is C8H11N, 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.

EXAMPLE 1 Bis(bis(trimethylsilyl)amido)bis(2,3,5-collidine)magnesium A 100-mL Schlenk flash was charged with bis(bis(trimethylsilyl)amido)bis(tetrahydrofuran)-magnesium (0.200 g, 0.460 mmol), a magnetic stir bar, and benzene (40 mL). 2,3,5-collidine (0.12 g, 0.91 mmol) was then added to this solution. The mixture was stirred for 18 h at room temperature. The volatile components were removed at reduced pressure to afford a yellow-orange solid. This solid was extracted into hexane (10 mL) and the resultant solution was filtered through a 2-cm pad of Celite.(R).. The filtrate was cooled to -20° C. for 18 h to afford colorless blocks of 1 (0.18 g, 66percent). Spectroscopic and analytical data for 1: mp 72°-73° C.; IR (Nujol, cm-1) 1249 (s), 1211 (m), 1148 (m), 1021 (s), 973 (s), 887 (s), 841 (s), 782 (s), 738 (s), 725 (s), 661 (s), 610 (s), 537 (s); 1 H NMR (C6 D6, delta) 8.39 (s, 2,3,5-collidine C-H), 6.63 (s, 2,3,5-collidine C-H), 2.43 (s, 2,3,5-collidine CH3), 1.81 (s, 2,3,5-collidine CH3), 1.69 (s, 2,3,5-collidine CH3), 0.33 (s, Si(CH3)3); 13 C{1 H} NMR (C6 D6, ppm) 154.32 (s, 2,3,5-collidine C-CH3), 147.00 (s, 2,3,5-collidine C-H), 139.41 (s, 2,3,5-collidine C-H), 132.00 (s, 2,3,5-collidine C-CH3), 131.26 (s, 2,3,5-collidine C-CH3), 22.04 (s, 2,3,5-collidine C-CH3), 18.62 (s, 2,3,5-collidine C-CH3), 17.45 (s, 2,3,5-collidine C-CH3), 5.87 (s, Si (CH3)3); Anal. Calcd for C28 H58 MgN4 Si4: C, 57.25; H, 9.95; N, 9.54. Found: C, 56.25; H, 10.00; N, 9.61.

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 695-98-7, 2,3,5-Trimethylpyridine.

Reference:
Patent; Wayne State University; US5892083; (1999); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 695-98-7, 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. 695-98-7, name is 2,3,5-Trimethylpyridine, molecular formula is C8H11N, 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.

EXAMPLE 1 Bis(bis(trimethylsilyl)amido)bis(2,3,5-collidine)magnesium A 100-mL Schlenk flash was charged with bis(bis(trimethylsilyl)amido)bis(tetrahydrofuran)-magnesium (0.200 g, 0.460 mmol), a magnetic stir bar, and benzene (40 mL). 2,3,5-collidine (0.12 g, 0.91 mmol) was then added to this solution. The mixture was stirred for 18 h at room temperature. The volatile components were removed at reduced pressure to afford a yellow-orange solid. This solid was extracted into hexane (10 mL) and the resultant solution was filtered through a 2-cm pad of Celite.(R).. The filtrate was cooled to -20° C. for 18 h to afford colorless blocks of 1 (0.18 g, 66percent). Spectroscopic and analytical data for 1: mp 72°-73° C.; IR (Nujol, cm-1) 1249 (s), 1211 (m), 1148 (m), 1021 (s), 973 (s), 887 (s), 841 (s), 782 (s), 738 (s), 725 (s), 661 (s), 610 (s), 537 (s); 1 H NMR (C6 D6, delta) 8.39 (s, 2,3,5-collidine C-H), 6.63 (s, 2,3,5-collidine C-H), 2.43 (s, 2,3,5-collidine CH3), 1.81 (s, 2,3,5-collidine CH3), 1.69 (s, 2,3,5-collidine CH3), 0.33 (s, Si(CH3)3); 13 C{1 H} NMR (C6 D6, ppm) 154.32 (s, 2,3,5-collidine C-CH3), 147.00 (s, 2,3,5-collidine C-H), 139.41 (s, 2,3,5-collidine C-H), 132.00 (s, 2,3,5-collidine C-CH3), 131.26 (s, 2,3,5-collidine C-CH3), 22.04 (s, 2,3,5-collidine C-CH3), 18.62 (s, 2,3,5-collidine C-CH3), 17.45 (s, 2,3,5-collidine C-CH3), 5.87 (s, Si (CH3)3); Anal. Calcd for C28 H58 MgN4 Si4: C, 57.25; H, 9.95; N, 9.54. Found: C, 56.25; H, 10.00; N, 9.61.

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 695-98-7, 2,3,5-Trimethylpyridine.

Reference:
Patent; Wayne State University; US5892083; (1999); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 695-98-7, 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. 695-98-7, name is 2,3,5-Trimethylpyridine, molecular formula is C8H11N, 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.

The yield of the product 2,3,5-collidine obtained from 3,5-lutidine used as a starting material was 86percent, and that of 2,3,5,6-tetramethylpyridine obtained therefrom was 3.4percent. The selectivities of the above-mentioned products were 96.3percent and 3.7percent, respectively.

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 695-98-7, 2,3,5-Trimethylpyridine.

Reference:
Patent; Koei Chemical Co., Ltd.; US4658032; (1987); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem