Category: 1003-73-2

Synthetic Route of 1003-73-2, 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. 1003-73-2, name is 3-Methylpyridine 1-oxide, molecular formula is C6H7NO, 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.

Into the flask, 300 g of methylene chloride and 50 g of 3-picoline-N-oxide were added and the mixture was stirred and cooled to 5°C at a constant pressure.A dropping funnel was charged with a mixed solution of 240 g of 2,4,6-triisopropyl-3-benzoyl chloride and 200 g of methylene chloride and slowly added dropwise to the dichloromethane mixture of 3-picoline-N-oxide. In the dropping process, the reaction temperature is controlled at 5 to 10°C.The addition was completed within about 3 hours. The reaction was incubated for 2 hours and then warmed to 40°C overnight.After the end of the reaction, cool down to 5 ~ 10 °C, slowly add 200g of water, after desolvation steam distillation, collecting 100 ~At 102°C/760mmHg, the distillate was extracted with methylene chloride. After the aqueous layer was separated, 57.4 g of product was de-solvated.The content of 2-chloro-5-methylpyridine was 98percent, 2-chloro-3-methylpyridine was 0.5percent, and the yield of 2-chloro-5-methylpyridine was 96.2percent.

According to the analysis of related databases, 1003-73-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Nanjing Hong Sun Biochemical Co., Ltd.; Chen Honglong; Mu Dengyou; Xue Yi; Chen Xinchun; Zhong Jingsong; Wang Fujun; Yang Cheng; (5 pag.)CN107721912; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 1003-73-2, name is 3-Methylpyridine 1-oxide, molecular formula is C6H7NO, 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. category: pyridine-derivatives

PREPARATION EXAMPLE 3 2-Chloro-5-methyl-pyridine A solution of 20 g (0.1 mol) of N,N-dipropylsulphamoyl chloride in 60 ml of chlorobenzene is added dropwise under nitrogen to a solution of 5.5 g (50 mmol) of 3-methylpyridine-1-oxide and 10.1 g (0.1 mol) of triethylamine in 40 mol of chlorobenzene. The mixture is then heated to 70° C. for a further 3 hours, the solid is then filtered off with suction, the filter cake is washed with chlorobenzene and the liquid phase is extracted using conc. hydrochloric acid.

With the rapid development of chemical substances, we look forward to future research findings about 1003-73-2.

Reference:
Patent; Bayer Aktiengesellschaft; US5099025; (1992); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 1003-73-2, name is 3-Methylpyridine 1-oxide. A new synthetic method of this compound is introduced below., Application In Synthesis of 3-Methylpyridine 1-oxide

Into the flask, 300 g of methylene chloride and 50 g of 3-picoline-N-oxide were added and the mixture was stirred and cooled to 5C at a constant pressure.A dropping funnel was charged with a mixed solution of 240 g of 2,4,6-triisopropyl-3-benzoyl chloride and 200 g of methylene chloride and slowly added dropwise to the dichloromethane mixture of 3-picoline-N-oxide. In the dropping process, the reaction temperature is controlled at 5 to 10C.The addition was completed within about 3 hours. The reaction was incubated for 2 hours and then warmed to 40C overnight.After the end of the reaction, cool down to 5 ~ 10 C, slowly add 200g of water, after desolvation steam distillation, collecting 100 ~At 102C/760mmHg, the distillate was extracted with methylene chloride. After the aqueous layer was separated, 57.4 g of product was de-solvated.The content of 2-chloro-5-methylpyridine was 98%, 2-chloro-3-methylpyridine was 0.5%, and the yield of 2-chloro-5-methylpyridine was 96.2%.

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, 1003-73-2, 3-Methylpyridine 1-oxide.

Reference:
Patent; Nanjing Hong Sun Biochemical Co., Ltd.; Chen Honglong; Mu Dengyou; Xue Yi; Chen Xinchun; Zhong Jingsong; Wang Fujun; Yang Cheng; (5 pag.)CN107721912; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 1003-73-2, Adding some certain compound to certain chemical reactions, such as: 1003-73-2, name is 3-Methylpyridine 1-oxide,molecular formula is C6H7NO, 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 1003-73-2.

PREPARATION EXAMPLE 3 2-Chloro-5-methyl-pyridine A solution of 20 g (0.1 mol) of N,N-dipropylsulphamoyl chloride in 60 ml of chlorobenzene is added dropwise under nitrogen to a solution of 5.5 g (50 mmol) of 3-methylpyridine-1-oxide and 10.1 g (0.1 mol) of triethylamine in 40 mol of chlorobenzene. The mixture is then heated to 70 C. for a further 3 hours, the solid is then filtered off with suction, the filter cake is washed with chlorobenzene and the liquid phase is extracted using conc. hydrochloric acid.

According to the analysis of related databases, 1003-73-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Bayer Aktiengesellschaft; US5099025; (1992); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 1003-73-2, name is 3-Methylpyridine 1-oxide, molecular formula is C6H7NO, 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. Recommanded Product: 1003-73-2

Example 1; A. 3-Methyl-isonicotinonitrile.; To 3-methyl-pyridine 1 -oxide (15.90 g, 150 mmol) is added at 0 0C during 30 min. dimethylsulfate (15.60 mL). The resulting reaction mixture is stirred overnight at 40 0C. A solution of KCN (10.75 g, 165 mmol) in a mixture of EtOH/water 1 : 1 (120 mL) is added and the reaction mixture is stirred overnight at 40 0C. The reaction mixture is concentrated in vacuo and the residue is partitioned between EtOAc and water. The aqueous phase is extracted with EtOAc and the combined organic layers are dried over Na2SO4, filtered and concentrated at reduced pressure. Purification by flash column chromatography (silica gel, cyclohexane / EtOAc 85 : 15) affords the title compound as orange crystals (6.00 g, 50.80 mmol, 34%). 1H NMR (400 MHz, DMSO-(Z6) delta ppm 8.76 (s, 1 H), 8.64 (d, J = 4.9 Hz, 1 H), 7.80 (d, J = 4.9 Hz, 1 H).

With the rapid development of chemical substances, we look forward to future research findings about 1003-73-2.

Reference:
Patent; NOVARTIS AG; WO2008/122615; (2008); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem