Category: 120739-77-7

Synthetic Route of 120739-77-7, 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. 120739-77-7, name is N-((6-Chloropyridin-3-yl)methyl)ethanamine, molecular formula is C8H11ClN2, 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.

352.0 g of n-butyl acetate and 102.9 g of a 35% potassium carbonate aqueous solution were charged in a 1-L separable flask. The solution was cooled to 4C, 48.8 g of 1,1-dichloro-2-nitroethene (net weight 40.6 g) was added dropwise while stirring over 30 minutes, and 44.8 g of 2-chloro-5-(ethylaminomethyl)pyridine (net weight 44.4 g) was subsequently added dropwise over 3 hours. The reaction mixture was stirred at -4C for 15 minutes, 60.6 g of a 40% methyl amine solution was added dropwise over 3 hours, and the stirring was further continued for 4 hours. The obtained reaction mixture was warmed to 15C and extracted four times with 51.5 g, 40.3 g, 30.0 g, and 30.0 g of water, and the obtained four extracted aqueous layers were combined. The combined aqueous layer was extracted four times with 75.0 g of 5-ethyl-2-methylpiridine at 15C, and the obtained four extracted 5-ethyl-2-methylpyridine layers were combined (amount of the recovered aqueous layer 1, 247.8 g). After washing the combined 5-ethyl-2-methylpyridine layer with 50.0 g of a saturated sodium sulfate solution (amount of the recovered aqueous layer 2, 66.0 g), 800 g of n-heptane was added thereto and concentrated at 4.5 kPa, 25 to 35C until the amount of the residual solution was 345 g. 20.0 g of 5-ethyl-2-methylpyridine was added to the concentrated mass, and the mixture was maintained at 40C for 1 hour followed by filtration to remove insoluble matters. The obtained filtrate was flushed down with 10.0 g of 5-ethyl-2-methylpyridine to a 500-ml separable flask, the temperature was adjusted to 35C. Then 0.01 g of seed crystals of (1E)-N-[(6-chloro-3-pyridinyl)methyl]-N-ethyl-N’-methyl-2-nitro-1,1-ethenediamine was added and the mixture was cooled to 15C over 5 hours, and subsequently cooled at -10C over 10 hours for crystallization. The crystalline mass was further stirred at -10C for 3 hours and filtered (recovered filtrate amount, 304.1 g). The obtained crystals were washed with 300.0 g of n-butyl acetate which had been cooled to -10C (recovered washing amount, 305.9 g). The washed crystals were dried at 2.7 kPa, 40C for 4 hours to obtain 45.3 g of (1E)-N-[(6-chloro-3-pyridinyl)methyl]-N-ethyl-N’-methyl-2-nitro-1,1-ethenediamine at a content of 98.9%

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 120739-77-7, N-((6-Chloropyridin-3-yl)methyl)ethanamine.

Reference:
Patent; Sumitomo Chemical Company, Limited; EP2186802; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 120739-77-7, 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. 120739-77-7, name is N-((6-Chloropyridin-3-yl)methyl)ethanamine, molecular formula is C8H11ClN2, 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.

352.0 g of n-butyl acetate and 102.9 g of a 35% potassium carbonate aqueous solution were charged in a 1-L separable flask. The solution was cooled to 4C, 48.8 g of 1,1-dichloro-2-nitroethene (net weight 40.6 g) was added dropwise while stirring over 30 minutes, and 44.8 g of 2-chloro-5-(ethylaminomethyl)pyridine (net weight 44.4 g) was subsequently added dropwise over 3 hours. The reaction mixture was stirred at -4C for 15 minutes, 60.6 g of a 40% methyl amine solution was added dropwise over 3 hours, and the stirring was further continued for 4 hours. The obtained reaction mixture was warmed to 15C and extracted four times with 51.5 g, 40.3 g, 30.0 g, and 30.0 g of water, and the obtained four extracted aqueous layers were combined. The combined aqueous layer was extracted four times with 75.0 g of 5-ethyl-2-methylpiridine at 15C, and the obtained four extracted 5-ethyl-2-methylpyridine layers were combined (amount of the recovered aqueous layer 1, 247.8 g). After washing the combined 5-ethyl-2-methylpyridine layer with 50.0 g of a saturated sodium sulfate solution (amount of the recovered aqueous layer 2, 66.0 g), 800 g of n-heptane was added thereto and concentrated at 4.5 kPa, 25 to 35C until the amount of the residual solution was 345 g. 20.0 g of 5-ethyl-2-methylpyridine was added to the concentrated mass, and the mixture was maintained at 40C for 1 hour followed by filtration to remove insoluble matters. The obtained filtrate was flushed down with 10.0 g of 5-ethyl-2-methylpyridine to a 500-ml separable flask, the temperature was adjusted to 35C. Then 0.01 g of seed crystals of (1E)-N-[(6-chloro-3-pyridinyl)methyl]-N-ethyl-N’-methyl-2-nitro-1,1-ethenediamine was added and the mixture was cooled to 15C over 5 hours, and subsequently cooled at -10C over 10 hours for crystallization. The crystalline mass was further stirred at -10C for 3 hours and filtered (recovered filtrate amount, 304.1 g). The obtained crystals were washed with 300.0 g of n-butyl acetate which had been cooled to -10C (recovered washing amount, 305.9 g). The washed crystals were dried at 2.7 kPa, 40C for 4 hours to obtain 45.3 g of (1E)-N-[(6-chloro-3-pyridinyl)methyl]-N-ethyl-N’-methyl-2-nitro-1,1-ethenediamine at a content of 98.9%

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 120739-77-7, N-((6-Chloropyridin-3-yl)methyl)ethanamine.

Reference:
Patent; Sumitomo Chemical Company, Limited; EP2186802; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 120739-77-7 ,Some common heterocyclic compound, 120739-77-7, molecular formula is C8H11ClN2, 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.

(2): Synthesis of N-((6-chloropyridin-3-yl)methyl)-N-ethyl-1-(methylthio)-2- nitroethenamine To a 100 ml three necked round bottom flask was added N-((6-chloropyridin-3-yl)methyl)ethanamine (17.0 g, 0.1 mol), (2-nitroethene-1,1-diyl)bis(methylsulfane) (15.0 g, 0.09 mol), dry ethanol (50 mL). The mixture was refluxed. After completion, the reaction mixture was cooled to r.t. and concentrated under reduced pressure to obtain crude product as oil, which was purified by column chromatography to afford 5.3 g N-((6-chloropyridin-3-yl)methyl)-N-ethyl-1- (methylthio)-2-nitroethenamine in 18.5% yield. GC-MS: m/z (%)=242 ([M]+-46, 53), 227 (15), 213 (100), 169 (45), 155 (28), 141 (29), 126 (91), 90 (12).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,120739-77-7, its application will become more common.

Reference:
Patent; SHANGHAI SHENGNONG PESTICIDE CO., LTD.; EAST CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY; US2011/269751; (2011); 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. 120739-77-7, name is N-((6-Chloropyridin-3-yl)methyl)ethanamine, the common compound, a new synthetic route is introduced below. name: N-((6-Chloropyridin-3-yl)methyl)ethanamine

General procedure: This embodiment is basically the same as Embodiment 1, except that:Step 2, using 170 g (15%) sodium carbonate instead of 52 g (40%) potassium carbonate aqueous solution, 41.8 g (98%) 2-chloro-5-ethylaminomethylpyridine instead of 40% methylamine.As a result, 70.5 g of (E)-N-(2-chloro-5-thiazolylmethyl)-N-ethyl-N’-(6-chloro-3-pyridylmethyl)-N’-ethyl-2- Nitrovinylidene diamine, content 98.1%, yield 83.1%. _: 2 In a 500 mL four-necked flask, 35.1 g (89%) of 1,1-dichloronitroethylene (0.22 mol) and 150 mL of dichloromethane were added.Stirring was carried out to 0 to 10 C, and 36.2 g (98%) of 2-chloro-5-ethylaminomethylthiazole (0.2 mol) was added dropwise. After the addition, 52 g (40%) of potassium carbonate aqueous solution was added dropwise at this temperature. , keep warm for 2 hours,Sampling HPLC analysis of N-(2-chloro-5-thiazole) methyl-N-ethylamine conversion rate of 98% or more, adding 38.8g (40%) methylamine aqueous solution (0.5mol) at 5-10 C, plus Stir for 1 hour after finishing.The temperature was raised to 20 to 25 C for 2 hours, and the oil layer was separated and allowed to stand, and the aqueous layer was extracted with dichloromethane for 3 times.The oil layer was desolvated, and 70 g of ethyl acetate was added to the residue, stirred well, and cooled to 0 to 5 C for filtration.Drying to obtain 50 g of (E)-N-(2-chloro-5-thiazolylmethyl)-N-ethyl-N’-methyl-2-nitrovinylidene diamine, content 98%, yield 88.6% .

The synthetic route of 120739-77-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lianyungang Liben Crop Technology Co., Ltd.; Wu Hailin; Dong Junjie; Dai Zhanyong; Gong Jian; Li Datie; (6 pag.)CN107474022; (2017); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 120739-77-7, 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. 120739-77-7, name is N-((6-Chloropyridin-3-yl)methyl)ethanamine, molecular formula is C8H11ClN2, 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.

2): Synthesis of N-(6-chloropyridin-3-yl)methylene)-N-ethyl-1-(methylthio)-2-nitrovinylidene amine To a 100 ml three necked round bottom flask, N-(6-chloropyridin-3-yl-methylene)ethylamine (17.0 g, 0.1 mol), 1,1-bis(methylthio)-2-nitroethene (15.0 g, 0.09 mol), anhydrous ethanol (50 mL) were added. The mixture was refluxed until full convention and cooled to r.t., The reaction was concentrated with reduced pressure to obtain a crude product as dense liquid, which was purified by column chromatography to yield 5.3 g N-(6-chloropyridin-3-yl-methylene)-N-ethyl-1-(methylthio)-2-nitrovinylidene amine in 18.5% yield.

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 120739-77-7, N-((6-Chloropyridin-3-yl)methyl)ethanamine.

Reference:
Patent; EAST CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY; US2010/298346; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 120739-77-7, 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 120739-77-7, name is N-((6-Chloropyridin-3-yl)methyl)ethanamine. This compound has unique chemical properties. The synthetic route is as follows.

1200 kg of dichloromethane was introduced into a 2000 L reactor, and 171 kg (1 kmol) of N-ethyl-2-chloro-5-pyridinemethylamine was added thereto with stirring, 60 L of ion exchange resin 201×7, and the mixture was cooled to an internal temperature of -10 C, and added dropwise. A solution of 157 kg (1.1 kmol) of 1-dichloro-2-nitroethylene and 320 kg of dichloromethane was added dropwise over 3 hours to control the internal temperature below 0 C. After the dropwise addition, the reaction was kept at 0 C for 3 hours. After the reaction is completed, a solution containing the compound (II) is obtained. The solution was further cooled to an internal temperature of -10 C, and slowly introduced into a methylamine gas of 46.5 kg, (1.5 kmol), controlled internal temperature of 0 C or less, and a calculated amount of monomethylamine gas was passed for 3 hours, and the temperature was maintained at 0 C. 3 hours. After completion, filtration, washing the ion exchange resin with dichloromethane, the filtrate is concentrated to dryness, adding 280 kg of ethyl acetate, stirring and crystallization at room temperature for 1 hour, then cooling to 0 C, stirring and crystallization for 3 hours, centrifuging the feed, drying to obtain the acetamid The amine was 252.3 kg, the purity was 99% or more, and the yield was 93%

According to the analysis of related databases, 120739-77-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanghai Jinjing Chemical Co., Ltd.; Chen Xuejun; Ma Jun; Tang Songqing; (6 pag.)CN108822025; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 120739-77-7 ,Some common heterocyclic compound, 120739-77-7, molecular formula is C8H11ClN2, 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.

To a 100ml three necked round bottom flask was added N-((6-chloropyridin-3-yl)methyl)ethanamine (17.0 g, 0.1 mol), (2-nitroethene-1,1-diyl)bis(methylsulfane) (15.0 g, 0.09 mol), dry ethanol (50 mL). The mixture was refluxed. After completion, the reaction mixture was cooled to r.t. and concentrated under reduced pressure to obtain crude product as oil, which was purified by column chromatography to afford 5.3g N-((6-chloropyridin-3-yl)methyl)-N-ethyl-1- (methylthio)-2-nitroethenamine in 18.5% yield. GC-MS: m/z (%) = 242 ([M]+-46, 53), 227 (15), 213 (100), 169 (45), 155 (28), 141 (29), 126 (91),90 (12).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,120739-77-7, its application will become more common.

Reference:
Patent; East China University of Science and Technology; Shanghai Shengnong Pesticide Co., Ltd.; EP2377845; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 120739-77-7 ,Some common heterocyclic compound, 120739-77-7, molecular formula is C8H11ClN2, 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.

To a 100ml three necked round bottom flask was added N-((6-chloropyridin-3-yl)methyl)ethanamine (17.0 g, 0.1 mol), (2-nitroethene-1,1-diyl)bis(methylsulfane) (15.0 g, 0.09 mol), dry ethanol (50 mL). The mixture was refluxed. After completion, the reaction mixture was cooled to r.t. and concentrated under reduced pressure to obtain crude product as oil, which was purified by column chromatography to afford 5.3g N-((6-chloropyridin-3-yl)methyl)-N-ethyl-1- (methylthio)-2-nitroethenamine in 18.5% yield. GC-MS: m/z (%) = 242 ([M]+-46, 53), 227 (15), 213 (100), 169 (45), 155 (28), 141 (29), 126 (91),90 (12).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,120739-77-7, its application will become more common.

Reference:
Patent; East China University of Science and Technology; Shanghai Shengnong Pesticide Co., Ltd.; EP2377845; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 120739-77-7, N-((6-Chloropyridin-3-yl)methyl)ethanamine, 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, 120739-77-7, blongs to pyridine-derivatives compound. category: pyridine-derivatives

1, In the 5000L stainless steel reactor,put disodium hydrogenphosphate 284kg, sodium dihydrogen phosphate, 67.9kg,720kg of tap water was added. Stirred solution becomes clear. At 25 deg.C, then 1500kg of methylene chloride was added, as well as N- (6-chloro – 3-pyridylmethyl) -N- ethylamine 341kg. Cooled 0 deg. C;2, was added dropwise 325 kg of 1,1-dichloro-2-nitroethylene, about 2 ~ 3h, temperature 5 ~ 10 deg.C;3, addition was complete at 5 ~ 10 deg.C. Maintain temperature for 2h; 4, then dropping 40% monomethylamine 390kg,about 2 ~ 3h, and maintain temperature for 2h at 5 ~ 10 deg.C ;5, then heated to 30 deg.C and hold temperature 1h; 6, still 30min, separated and the aqueous layer was further 500kg, extracted once with methylene chloride; 7, the combined organic phases, first at atmospheric pressure and then vacuum recovery methylene chloride, ethyl acetate500kg;8, 0 ~ 5 deg.C cooling crystallization 2h, centrifugal drying drying material, was 494.1kg, HPLC?99.5%,external standard content ?98%, a yield of 0.92.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,120739-77-7, its application will become more common.

Reference:
Patent; Shanghai Jinjing Chemical Co., Ltd.; Long, Congwei; Ma, Jun; Zhou, Xianpei; Tang, Songqing; Lv, Yejun; (9 pag.)CN105330593; (2016); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 120739-77-7, 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. 120739-77-7, name is N-((6-Chloropyridin-3-yl)methyl)ethanamine. A new synthetic method of this compound is introduced below.

EXAMPLE 12 A solution of 2.4 g (0.014 mol) of N-(6-chloro-3-pyridyl)methyl-N-ethylamine, 1.4 g (0.014 mol) of triethylamine in 5 ml of acetonitrile was dropwise added to a solution of 2.0 g (0.014 mol) of 1,1-dichloro-2-nitroethylene in 35 ml of acetonitrile at 3-5 C. with stirring. After stirring for 30 minutes, 4.4 g (0.057 mol) of methylamine (40% methanol solution) were added to the reaction mixture and stirred for 30 minutes. The reaction mixture was filtered, and the filtrate was concentrated and purified by a silica gel column chromatography (chloroform/ethanol=7/1) to afford 2.9 g (76.5%) of 1-[N-(6-chloro-3-pyridyl)methyl-N-ethyl]amino-1-methylamino-2-nitroethylene as pale yellowish crystals.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,120739-77-7, its application will become more common.

Reference:
Patent; Takeda Chemical Industries, Ltd.; US5364989; (1994); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem