Category: 39856-50-3

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. 39856-50-3, name is 5-Bromo-2-nitropyridine, the common compound, a new synthetic route is introduced below. Product Details of 39856-50-3

Method- 1Piperazine (85 g) and 5-Bromo-2-nitropyridine (100 g) were added in DMF and cooled to 50-60C, followed by addition of 2-propanol (1000 ml) and stirred for 1 hr. The reaction mixture was further cooled to 20-30C and stirred for 2-3 hrs. The reaction mass was filtered under vacuum and washed with 2-propanol. The resulting solid was treated with Boc anhydride (161 g) in the presence of diisopropyl ethyl amine (95 g) in dichloromethane (500 ml) at ambient temperature. Product was isolated by addition of n-heptane (1200 mL) followed by filtration and washing with n-heptane and dried under vacuum at 50-60C to give pale yellow solid (130 g).Yield: 85.0 %; HPLC Purity: 99.0%

The synthetic route of 39856-50-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FRESENIUS KABI ONCOLOGY LTD.; SOKHI, Sarbjot Singh; SINGH, Govind; LAHIRI, Saswata; PANDEY, Maneesh Kumar; TIWARI, Raj Narayan; SHUKLA, Sonu; MUSMADE, Sachin; DUA, Heena; CABRI, Walter; (70 pag.)WO2019/82143; (2019); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 39856-50-3 ,Some common heterocyclic compound, 39856-50-3, molecular formula is C5H3BrN2O2, 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.

Under a nitrogen purge, the solid 4-bromo-2-nitropyridine (10. Ig; 0.05mol), potassium carbonate (10.5g; 0.075mol; -325mesh), tetrabutylammonium iodide (1.25g; 5mol%), and piperazine (5.4g; 0.0625mol) were sequentially added to 80ml acetonitrile. The suspension was heated to reflux, and maintained for 16 h. The now-bright yellow suspension was filtered hot, and the filter cake washed with a few portions of hot acetonitrile, such that the filtrate flows only slightly yellow. The filtrate quickly deposited a yellow/orange solid. This was reheated to obtain a clear solution, which was placed in the refrigerator for 16 h. The yellow/orange solid was isolated by filtration and the filter cake was washed with small portion cold CH3CN, followed by a small portion of petroleum ether. Air drying the solid provided ca 10.2g of solid material, about 65% of theory. Another 2g of material was isolated by evaporating the acetonitrile filtrate down to a semi-solid and then recrystallizing the residue from a minimum amount of hot isopropanol (treated with activated charcoal). NMR: 1.63 (s, IH), 2.99 (m, 4H), 3.36 (m, 4H), 7.14 (m, IH), 8.08 (m, 2H), m/z 209.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 39856-50-3, 5-Bromo-2-nitropyridine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/95159; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 39856-50-3, 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.39856-50-3, name is 5-Bromo-2-nitropyridine, molecular formula is C5H3BrN2O2, molecular weight is 202.99, as common compound, the synthetic route is as follows.

To a solution of compound (1) (20.00 g, 98.53 mmol, 1.00 eq) in dimethyl sulfoxide (52 mL), compound (2) (24.00 g, 128.86 mmol, 1.31 eq) and triethylamine (20.00 g, 197.65 mmol, 2.01 eq) were added. The solution was heated to 60 C. and stirred for 18 hours. TLC (petroleum ether:ethyl acetate=3:1) showed the completion of the reaction. The solution was diluted with water (200 mL), stirred for 30 minutes, and then filtered. The filter cake was washed with water and dried under vacuum to obtain a crude product. The crude product was purified by a silica gel column (petroleum ether:ethyl acetate=50:1 to 20:1) to obtain compound (3) (27.00 g, 87.57 mmol, yield: 88.87%). 1H NMR (400 MHz, CDCl3) delta8.18 (d, J=9.03 Hz, 1H), 8.13 (d, J=2.89 Hz, 1H), 7.21 (dd, J=9.10, 2.95 Hz, 1H), 3.69-3.59 (m, 4H), 3.51-3.40 (m, 4H), 1.49 (s, 9H).

The chemical industry reduces the impact on the environment during synthesis 39856-50-3, I believe this compound will play a more active role in future production and life.

Reference:
Patent; CHIA TAI TIANQING PHARMACEUTICAL GROUP CO., LTD.; Ding, Charles Z.; Chen, Shuhui; Hu, Lihong; Xu, Zhaobing; Liu, Yingchun; Ren, Bingjie; Li, Weidong; Li, Zongbin; Zhao, Rui; Zhang, Xiquan; (21 pag.)US2019/194168; (2019); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 39856-50-3, 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 39856-50-3, name is 5-Bromo-2-nitropyridine. This compound has unique chemical properties. The synthetic route is as follows.

Into a solution of 5-bromo-2-nitropyridine (30 g, 148 mmol) in DMSO (1 L) were added K2CO3 (40 g, 296 mmol) and teri-butyl piperazine-l-carboxylate (28g, 148 mmol). The mixture was stirred at 65 degree for overnight. After cooling down, it was poured into water (2 L). The solid precipitated was collected and dried under vacuum. It was then further purified by flash column eluting with 20:1 petroleum ether/ethyl acetate and then with methylene chloride to give 188a as a yellow solid (17 g, 37%). MS: [M+H]+ 309.

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 39856-50-3, 5-Bromo-2-nitropyridine.

Reference:
Patent; GILEAD CONNECTICUT, INC.; GENENTECH, INC.; BARBOSA, Antonio, J., M.; BLOMGREN, Peter, A.; CURRIE, Kevin, S.; KRISHNAMOORTHY, Ravi; KROPF, Jeffrey, E.; LEE, Seung H.; MITCHELL, Scott A.; ORTWINE, Daniel; SCHMITT, Aaron, C.; WANG, Xiaojing; XU, Jianjun; YOUNG, Wendy; ZHANG, Honglu; ZHAO, Zhongdong; ZHICHKIN, Pavel E.; WO2011/140488; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 39856-50-3 ,Some common heterocyclic compound, 39856-50-3, molecular formula is C5H3BrN2O2, 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.

1) 5-Bromo-2-nitropyridine (1 mol, 203 g) was dissolved in 1.5 L of dimethyl sulfoxide, and then an organically modified hectorite-supported ionic liquid material MHIL (40.6 g, 20 wt%) was added. Agitating and dispersing uniformly to obtain a first mixed liquid;2) Piperazine (129.2 g, 1.5 mol) was dissolved in 800 ml of dimethyl sulfoxide to form a piperazine solution, and then the piperazine solution was added dropwise to the first mixture to carry out a condensation reaction at 80 C;3) After 5 hours, the reaction solution was taken for HPLC detection (the percentage of 5-bromo-2-nitropyridine in the reaction solution was 0.08%, and the target product 1-(6-nitropyridin-3-yl)piperazine was 99.68%. Double condensation by-product 0.17%, the balance is unknown impurities), stop the reaction, use an organic microporous membrane with a pore size of 0.5 mum to filter and remove the organic modified hectorite-loaded ionic liquid material to obtain a filtrate;4) The filtrate is warmed to 60-65 C, and then the aqueous solution of methylamine at a concentration of 3 V% is added dropwise. When the turbidity occurs in the system, the dropwise addition is stopped, the mixture is kept warm for 20-30 min, and then the aqueous solution of methylamine having a concentration of 3 V% is continuously added dropwise. The concentration of 1-(6-nitropyridin-3-yl)piperazine in the solution was no longer decreased, and the temperature was naturally lowered to room temperature, filtered, and dried under vacuum at 45 C to obtain 197.4 g of a solid. The yield was 94.8%. 99.92% (external standard method); LC-MS: m/z = 209.1 [M+H].The ionic liquid material supported by the organic modified hectorite filtered by filtration was air-dried by acetone and recovered, and the yield of 1-(6-nitropyridin-3-yl)piperazine was 94.2%, and the content was 99.89%. Compared with the catalytic effect of fresh preparation, the catalytic material prepared by the invention can be recycled and used to reduce the production cost of the condensation step.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,39856-50-3, its application will become more common.

Reference:
Patent; Zheng Chuanhua; Lu Xueling; Zhang Lei; (10 pag.)CN109369517; (2019); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 39856-50-3, 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 39856-50-3, name is 5-Bromo-2-nitropyridine. This compound has unique chemical properties. The synthetic route is as follows.

Piperazine-1 -carboxylic acid tert- butyl ester (3.0 g, 16.11 mmol), 5-bromo-2-nitro-pyridine (3.3 g, 16.11 mmol) and DIPEA (6.2 g, 48.32 mmol) in ethanol (30 ml.) are stirred at rt for 20 h. The reaction mixture is concentrated under reduces pressure and the residue is diluted with ethyl acetate and water. The organic layer is washed with water, brine, dried over MgS04, filtered and concentrated under reduces pressure. The residue is purified with column chromatography using silica gel (EtOAc/heptane) to afford the title compound. (0485) Yield: 1.34 g (27%) ESI-MS: m/z = 309 (M+H)+ Rt(HPLC): 0.89 min (Method 1

According to the analysis of related databases, 39856-50-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; HYDRA BIOSCIENCES, INC.; BRUNETTE, Steven; CUI, Jianwen; LOWE, Michael D.; SARKO, Christopher Ronald; SURPRENANT, Simon; TURNER, Michael Robert; WU, Xinyuan; SMITH KEENAN, Lana Louise; BOUYSSOU, Thierry; (183 pag.)WO2019/158572; (2019); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 39856-50-3, 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.39856-50-3, name is 5-Bromo-2-nitropyridine, molecular formula is C5H3BrN2O2, molecular weight is 202.99, as common compound, the synthetic route is as follows.

To a solution of 5-bromo-2-nitropyridine (40.0 g,197 mmol) in DMSO (150 mL) were added 1-Bocpiperazine(47.4 g, 252 mmol) and DIPEA (38 mL,219 mmol) . The reaction mixture was heated at 80 C for11 h. The reaction mixture was poured into ice-water andthen extracted with EtOAc. The combined extracts werewashed with water and brine. The organic layer was driedover Na2SO4, filtered, and concentrated under reducedpressure. Purification by column chromatography (1:9methanol/ dichloromethane) gave 1-Boc- 4-(6-nitro-pyridin-3-yl)-piperazine (49.9 g, 82%) as yellow solid. 1H NMR(400 MHz, CDCl3): delta 8.11 (d, J = 9.1 Hz, 1H), 8.08 (d, J =2.7 Hz, 1H), 7.18 (dd, J = 9.1, 2.8 Hz, 1H), 3.65-3.56 (m,4H), 3.48-3.38 (m, 4H), 1.45 (s, 9H).

Statistics shows that 39856-50-3 is playing an increasingly important role. we look forward to future research findings about 5-Bromo-2-nitropyridine.

Reference:
Article; Guo, Qingxiang; Li, Yongtao; Zhang, Chao; Huang, Zhi; Wang, Xin; Nie, Yongwei; Li, Yao; Liu, Yanhua; Yang, Shengyong; Xiang, Rong; Fan, Yan; Medicinal Chemistry Research; vol. 27; 6; (2018); p. 1666 – 1678;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 39856-50-3, Adding some certain compound to certain chemical reactions, such as: 39856-50-3, name is 5-Bromo-2-nitropyridine,molecular formula is C5H3BrN2O2, 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 39856-50-3.

Preparation XX Synthesis of 4-r6-amino-pyridin-3-ylVpiperazine-l-carboxylic acid tert-butyl ester Step 1. Synthesis of 4-f6-nitro-pyridin-3-yl)-piperazine-l-carboxyric acid tert-butyl ester; A mixture of 5-bromo-2-nitropyridine (4.93g, 24.30 mmol) and tert-butyl piperazine-1-carboxylate (5.Og, 26.7 mmol) in acetonitrile (60ml) was heated at refluxed for 3 days. The solvent was evaporated and the solid residue purified by flash chromatography on silica eluting with EtO Ac/Petrol (1:3) and recrystallised from EtO Ac/Petrol to afford the title compound as an orange solid (5.Og, 67%) (LCMS: Rt 2.8, [M+H]+ 309).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 39856-50-3, 5-Bromo-2-nitropyridine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTEX THERAPEUTICS LIMITED; NOVARTIS AG; WO2008/7123; (2008); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 39856-50-3, 5-Bromo-2-nitropyridine, 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-Bromo-2-nitropyridine, blongs to pyridine-derivatives compound. Recommanded Product: 5-Bromo-2-nitropyridine

Step A: 1-(6-Nitropyridin-3-yl)piperazine Under a protection of nitrogen, to a solution of piperazine (2.55g, 29.56mmol) and 5-bromo-2-nitro-pyridine (5g, 24.63mmol) in acetonitrile (40mL) were added potassium carbonate (5.11g, 36.95mmol) and tetrabutylamine iodide (636.83mg, 1.72mmol) and it was stirred at 100C for 16 hours. It was immediately filtered at a high temperature, and the filter cake was washed with hot acetonitrile, followed by a precipitating of solid from the filtrate, filtration again. The filter cake was washed with a small portion of cold acetonitrile, then spin-dried to give the title compound. MS-ESI (m/z): 209(M+1). 1H NMR (400MHz, DMSO-d6) delta=8.23 (d, J=3.0 Hz, 1H), 8.13 (d, J=9.3 Hz, 1H), 7.44 (dd, J=3.0, 9.3 Hz, 1H), 3.43-3.38 (m, 4H), 2.87-2.76 (m, 4H).

The synthetic route of 39856-50-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chia Tai Tianqing Pharmaceutical Group Co., Ltd.; LIU, Shilan; LIANG, Guibai; WANG, Hongjian; ZHANG, Ming; CHEN, Shuhui; (93 pag.)EP3640247; (2020); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem