Day: September 24, 2021

Synthetic Route of 499-51-4, 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 499-51-4 as follows.

A mixture of 205 4-hydroxypyridine-2,6-dicarboxylic acid 18a (10 g, 54.6 mmol), 206 phosphorus pentachloride (56 g, 272 mmol) and 179 chloroform (30 mL) was heated to 80 C. and stirred for three days. The mixture was cooled to room temperature and added slowly with 31 methanol (20 mL). The obtained mixture was stirred at room temperature for 2 h, basified with a solution of 118 sodium bicarbonate and extracted with dichloromethane (50 mL). The organic phase was combined, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography to give the target 207 compound dimethyl 4-chloropyridine-2,6-dicarboxylate 18b (8 g, white solid). Yield: 64%. MS m/z (ESI): 230[M+1]

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,499-51-4, its application will become more common.

Reference:
Patent; Beijing Innocare Pharma Tech Co., Ltd.; CHEN, Xiangyang; GAO, Yingxiang; US2019/185472; (2019); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 55717-45-8, Adding some certain compound to certain chemical reactions, such as: 55717-45-8, name is 6-Bromopyridin-3-ol,molecular formula is C5H4BrNO, 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 55717-45-8.

2-Bromo-5-hydroxypyridine (5 mmol) is dissolved in DMF (10 ml) and NaH (1.4 eq., 60% suspension in liquid paraffin) is added. After 30 min iodomethane (2 eq.) is added and the reaction solution is stirred 3 days. The reaction solution is pored into water and extracted with methyl-tert-15 butyl ether. The combined organic layers are dried over MgSO4 and the solvent is removed in vacuo. 2-Bromo-5-methoxy-pyridine is obtained as yellow oil in a yield of 79 %; HPLC (method C): 1.49 min; LC-MS (method A): 1.16 min, 187.95 (M+H+).

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. 55717-45-8, 6-Bromopyridin-3-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK PATENT GMBH; WO2009/46784; (2009); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 159503-91-0, name is tert-Butyl 4-bromo-5,6-dihydropyridine-1(2H)-carboxylate. This compound has unique chemical properties. The synthetic route is as follows. Formula: C10H16BrNO2

In the third step, a Grignard exchange reaction of 26.21 g (0.1 mol) of N-Boc piperidin-4-enyl bromide with 12.9 g (0.105 mol) of isopropyl bromide in tetrahydrofuran, and then, under the protection of nitrogen, At 0 C, 19.03 g (0.11 mol) of pinacol methoxyboronic acid was added dropwise to the Grignard reaction solution, the reaction was held for 4 h, and then the temperature was raised to reflux for 1 h. After the reaction was completed, 10 ml of 10% dilute hydrochloric acid was added to quench the reaction. After the solvent was distilled off, 120 ml of ethanol was added for beating. The white solid was filtered to obtain 26.9 g, and the yield was 87%.

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, 159503-91-0, tert-Butyl 4-bromo-5,6-dihydropyridine-1(2H)-carboxylate.

Reference:
Patent; Zhonghao (Dalian) Chemical Design Yuan Co., Ltd.; Wang Kewei; Cai Xiaochuan; Zhao Wenwu; Tang Peikun; Han Jianguo; (6 pag.)CN110526936; (2019); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 82671-06-5, 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 82671-06-5 as follows.

In a round-necked flask 2,6-dichloro-5-fluoro-nicotinic acid (20.0g, 95.2mmol), sodium methoxide (11.3g, 210mmol) and anhydrous methanol (with 260 mL of), the reaction was refluxed for 4 hours, cooled to at room temperature, was added 200mL of water, acidified with concentrated hydrochloric pH = 1, then extracted with ethyl acetate, dried over anhydrous Na2SO4Dried, the solvent was spin-product 19.0g, a yield of 97.4%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,82671-06-5, its application will become more common.

Reference:
Patent; Shandong Xuanzhu Pharmaceutical Technology co., LTD; WU, YONG QIAN; WANG, AI CHEN; (35 pag.)CN102887895; (2016); B;,
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. 1180132-17-5, name is 5-((4-Ethylpiperazin-1-yl)methyl)pyridin-2-amine, the common compound, a new synthetic route is introduced below. Recommanded Product: 1180132-17-5

Compound 8a (216 mg, 0.7 mmol), compound 12 (154 mg, 0.7 mmol), sodium carbonate (74 mg, 0.7 mmol), 4 5-bisdiphenylphosphino-9 9-dimethyloxanthene (Xantphos) , 121 mg, 0.21 mmol) dissolved in 1,4-dioxane (20 mL), added with palladium acetate (16 mg, 0.07 mmol) under nitrogen atmosphere, reacted at 90 C for 10 hours, and the reaction solution was cooled to room temperature. into 50 mL of water, extracted three times with dichloromethane (30mL x3), the organic phases were combined, dried over anhydrous sodium sulfate filtered, and spin dry solid was recrystallized from ethyl acetate to give a yellow solid T-1 (150 mg, 44%) .

The synthetic route of 1180132-17-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hangzhou Bai Cheng Pharmaceutical Technology Co., Ltd.; Sheng Rong; Lou Jinfang; Zhang Fengmin; Luo Jin; Wu Lijun; Yang Huan; Jin Zewu; Xiong Xiaohong; Qian Yang; (32 pag.)CN110156754; (2019); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 99368-67-9, 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. 99368-67-9, name is 2-Chloro-5-nitro-3-(trifluoromethyl)pyridine. A new synthetic method of this compound is introduced below.

Reference Example 119 6-chloro-5-(trifluoromethyl)pyridine-3-amine; Reduced iron (1.3 g) and ammonium chloride (2.1 g) were added to water (40 mL), and the mixture was stirred at room temperature for 5 min. A solution of 2-chloro-5-nitro-3-(trifluoromethyl)pyridine (1.8 g) in methanol (40 mL) was added, and the mixture was stirred at room temperature for 1 hr. Reduced iron (2.3 g) was added, and the mixture was further stirred at the same temperature for 3 hr. The reaction mixture was filtered through celite, and celite was washed with ethyl acetate. The filtrate was extracted with ethyl acetate, and the extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=19:1?1:1) to give the title compound as a solid (yield 1.0 g, 65%). 1H-NMR (CDCl3) delta: 7.29 (1H, m), 7.99 (1H, m), 2H not detected.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,99368-67-9, 2-Chloro-5-nitro-3-(trifluoromethyl)pyridine, and friends who are interested can also refer to it.

Reference:
Patent; Takeda Pharmaceutical Company Limited; US2007/60623; (2007); 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. 1603-41-4, name is 2-Amino-5-methylpyridine, the common compound, a new synthetic route is introduced below. Recommanded Product: 1603-41-4

3.40 mL of 50% sulfuric acid (v / v) was added to a 25 mL reaction flask followed by the addition of 1.00 g (10 mmol) of 2-amino-5-methylpyridine (Compound 1), the ice salt bath was cooled to below 10 C, After a few minutes, the reaction solution became milky white; and then slowly slowly adding 1.72 g (25 mmol) of a mixture of NaNO2 and 3 mL of H2O to form a brownish-colored irritating odor gas, and the reaction solution Into a pale yellow, with 10% dilute sulfuric acid to adjust the pH to 7-8, reflux stirring reaction about 20min, spin off most of the water, to which the appropriate amount of 300 mesh silica gel, spin dry, into the glass sand core funnel, The ester was filtered and the filtrate was spin-dried to obtain the crude product (Compound 3) which was used in the next step without purification.

The synthetic route of 1603-41-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan University; Yin, Shu-Fan; Li, Yong; Cao, Tingting; Yang, Ziyao; (16 pag.)CN105998016; (2016); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 6602-32-0, 2-Bromo-3-hydroxypyridine, 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, Quality Control of 2-Bromo-3-hydroxypyridine, blongs to pyridine-derivatives compound. Quality Control of 2-Bromo-3-hydroxypyridine

Diethyl azodicarboxylate (95 mL, 0.6 mol) was added dropwise to a stirred mixture of 2-bromo-3- hydroxypyridine (97 g, 0.55 mol), 3-buten-l-ol (47.7 mL, 0.55 mol), and PPh3 (175.3 g, 0.66 mol) in THF (970 mL) at 0C under a N2 atmosphere. The reaction mixture was warmed to 50C in an oil bath and stirred for 17.5 h. Reaction progress was monitored by TLC (15% EtOAc in hexane, UV active). The reaction mixture was cooled to ambient temperature and diluted with saturated NaHC03 solution (500 n L). The aqueous solution was extracted with EtOAc (1 L). The organic layer was dried over Na2S04 (200 g), and concentrated. The residual product was purified by column chromatography using 60-120 mesh, eluting with 5% EtOAc in hexane to afford the title compound as a pale yellow oil. MS (ESI) m/z; 228 (MH+).

The synthetic route of 6602-32-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NANT HOLDINGS IP, LLC; NANTWORKS, LLC; TAO, Chunlin; WANG, Qinwei; SOON-SHIONG, Patrick; (94 pag.)WO2017/24315; (2017); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 104408-23-3 ,Some common heterocyclic compound, 104408-23-3, molecular formula is C5H5Cl2N3, 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.

STR93 (Process (a) 16.9 g (0.1 mole) of ethyl ethoxymethylenecyanoacetate and 17.8 g (0.1 mole) of 3,5-dichloro-pyrid-2-ylhydrazine in 150 ml of ethoxyethanol are stirred at 80 C. for 5 hours and then at 120 C. for a further 2 hours. For working up, the solvent is removed in vacuo. 29.6 g (98% of theory) of 5-amino-1-(3,5-dichloro-pyrid-2-yl)-4-ethoxycarbonyl-pyrazole of melting point 98-101 C. are obtained.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,104408-23-3, its application will become more common.

Reference:
Patent; Bayer Aktiengesellschaft; US4772312; (1988); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 106877-33-2, name is 5-Amino-2-(trifluoromethyl)pyridine. This compound has unique chemical properties. The synthetic route is as follows. COA of Formula: C6H5F3N2

(1) Pyridine (2.9 mL) was added to a solution of 2-trifluoromethyl-5-aminopyridine (1.95 g) in chloroform (15 mL), the mixture was cooled in ice, and phenyl chloroformate (1.8 mL) was added thereto. The resulting mixture was stirred at room temperature overnight, and the reaction mixture was concentrated under reduced pressure. The residue was washed with isopropyl ether to afford phenyl[6-(trifluoromethyl)pyridin-3-yl]carbamate (2.16 g). (ESI pos.) m/z: 283 ([M+H]+)

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, 106877-33-2, 5-Amino-2-(trifluoromethyl)pyridine.

Reference:
Patent; TAISHO PHARMACEUTICAL CO., LTD; Moriya, Minoru; Ohta, Hiroshi; Yamamoto, Shuji; Abe, Kumi; Araki, Yuko; Sun, Xiang-Min; Wakasugi, Daisuke; US2013/331571; (2013); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem