Day: April 12, 2022

Related Products of 88912-24-7 ,Some common heterocyclic compound, 88912-24-7, molecular formula is C6H3Cl2NO2, 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.

EXAMPLE 12 2,3-bis(methylthio)pyridine In a 4-necked flask equipped with a Dry Ice condenser, mechanical stirrer, thermometer and dropping funnel, 172.2 g of t-BuOK was dissolved in 200 ml of DMSO at room temperature with stirring under N2. The solution was cooled with an ice bath while 50.0 g of methanethiol was added. The mixture was stirred for 30 minutes, then the ice bath was removed. A solution of 5,6-dichloro-2-pyridinecarboxylic acid (90.6 g) in 250 ml of DMSO was added at a rate such that the exotherm did not cause the temperature of the mixture to exceed 75 C. A dense slurry formed. An additional 500 ml of DMSO was added, and the slurry was stirred for 42 hours at 60 C. After cooling to room temperature, 500 ml of water was added to the reaction mixture, which was then added to 3.5 liters of ice water, and acidified to pH 1 with concentrated HCl. The yellow precipitate which formed was collected and dried which gave 87.33 g of a mixture of 5-chloro-6-(methylthio)-2-pyridinecarboxylic acid (~3.36 g) and 5,6-bis(methylthio)-2-pyridinecarboxylic acid (~83.97 g). The relative amounts of the 5-chloro-6-(methylthio)-2-pyridinecarboxylic acid and 5,6-bis(methylthio)-2-pyridinecarboxylic acid were estimated based on the amounts of the mono and bis-adducts isolated after decarboxylation.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,88912-24-7, its application will become more common.

Reference:
Patent; The Dow Chemical Company; US4616087; (1986); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 1026796-81-5, N-(4-Bromopyridin-2-yl)acetamide, 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, 1026796-81-5, blongs to pyridine-derivatives compound. COA of Formula: C7H7BrN2O

[00348] To a solution of N-(4-bromopyridin-2-yl)acetamide (350 mg, 1.6 mmol) in DCM (20 niL) was added mCPBA (1.26 g, 7.3 mmol) at 0C. The reaction mixture was allowed to stir at ii for 3 h. The reaction mixture was then diluted with water and saturated K2C03 solution, and extracted with DCM. The organic solutions were combined, dried over Na2SO4, filtered and concentrated. The crude compound was purified by column chromatography to provide N-(4-bromo-1-oxidopyridin-2- yl)acetamide (340 mg, 90%). LCMS (FA): m/z 231.3 (M+H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1026796-81-5, its application will become more common.

Reference:
Patent; MILLENNIUM PHARMACEUTICALS, INC.; BHARATHAN, Indu T.; BLACKBURN, Chris; CIAVARRI, Jeffrey P.; CHOUITAR, Jouhara; CULLIS, Courtney A.; D’AMORE, Natalie; FLEMING, Paul E.; GIGSTAD, Kenneth M.; GIPSON, Krista E.; GIRARD, Mario; HU, Yongbo; LEE, Janice; LI, Gang; REZAEI, Mansoureh; SINTCHAK, Michael D.; SOUCY, Francois; STROUD, Stephen G.; VOS, Tricia J.; WONG, Tzu-Tshin; XU, He; XU, Tianlin; YE, Yingchun; WO2015/108861; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 60781-83-1, 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. 60781-83-1, name is 4-Phenylpyridin-2-amine. A new synthetic method of this compound is introduced below.

EXAMPLE 8 2,3-Dihydro-6-phenylcyclopenta[d]pyrido[1,2-a]pyrimidin-10(1H)-one A mixture of 17.0 g. of 2-amino-4-phenylpyridine and 31.2 g. of ethyl cyclopentane-2-carboxylate is heated at an internal temperature of 160-165 for 4 hours. During this time ethanol distils from the reaction mixture and is collected in a Dean-Stark trap. During the 4 hours of heating, about 5.5 ml of distillate is collected. When the reaction mixture is allowed to cool, a crystalline solid separates. The mixture is cooled to 0 and the solid filtered. Recrystallization from cyclohexane gives 24.7 g. of 2,3-dihydro-6-phenylcyclopenta[d]pyrido[1,2-a]pyrimidin-10(1H)-one.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,60781-83-1, its application will become more common.

Reference:
Patent; E. R. Squibb & Sons, Inc.; US3965100; (1976); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 2897-43-0, 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.2897-43-0, name is 2,6-Dichloro-3-nitropyridin-4-amine, molecular formula is C5H3Cl2N3O2, molecular weight is 208, as common compound, the synthetic route is as follows.

(C) 2,6-dichloropyridi ne-3,4-diami ne[083] To a solution of 2,6-dichloro-3-nitropyridin-4-amine in ethanol (150 mL) was added iron powder (14.3 g, 0.255 mol), water (46 mL), and then concentrated HCI (28 mL). The reaction mixture was then stirred at 95 C for 16 hours, cooled to room temperature, and neutralized. The precipitates were collected by filtration and dried in vacuo. The crude product was then treated with water (200 mL) and extracted with EtOAc (3 x 200 mL). The combined extracts were dried over anhydrous Na2S04, filtered, and concentrated to afford 7.85 g of the title compound (86.5% yield).

Statistics shows that 2897-43-0 is playing an increasingly important role. we look forward to future research findings about 2,6-Dichloro-3-nitropyridin-4-amine.

Reference:
Patent; HUTCHISON MEDIPHARMA LIMITED; SU, Wei-Guo; DENG, Wei; JI, Jianguo; WO2012/167423; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 697739-12-1, Ethyl imidazo[1,5-a]pyridine-8-carboxylate, 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: 697739-12-1, blongs to pyridine-derivatives compound. Recommanded Product: 697739-12-1

Description 36 (8.67 g, 45.6 mmol) and KOH [1. OM in methanol] (91.2 ml, 91.2 mmol) were mixed together and heated to reflux for 30 minutes when HPLC indicated the reaction was complete. The mixture was cooled and evaporated to dryness. Water (50 ml) was then added, and the mixture acidified with 2N HC1 to give a yellow precipitate. The precipitate was filtered and washed successively with water, ethanol, and diethyl ether to give the title compound (3.1 g, 42%) as a yellow solid

At the same time, in my other blogs, there are other synthetic methods of this type of compound,697739-12-1, Ethyl imidazo[1,5-a]pyridine-8-carboxylate, and friends who are interested can also refer to it.

Reference:
Patent; Merck Sharp & Dohme Limited; WO2004/46133; (2004); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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 7477-10-3, name is 6-Chloro-5-nitronicotinic acid. This compound has unique chemical properties. The synthetic route is as follows. Safety of 6-Chloro-5-nitronicotinic acid

EXAMPLE 16 2-Fluoro-3- nitro-5-trifluoromethylpyridine/2-chloro-3-nitro-5-trifluoromethylpyridine mixture A steel bomb was charged with 6-chloro-5-nitronicotinic acid (4.1 g, 0.02 m), SF4 (21 g) and HF (3.7 ml). The mixture was heated at 90 for eight hours. After cooling to 25, the bomb was vented and the contents poured onto ice. The solution was neutralized with saturated Na2 CO3 solution and extracted with CH2 Cl2. The organic layer was dried over Na2 SO4, filtered and the solution was distilled. A mixture of 2-chloro and 2-fluoro-3-nitro-5-trifluoromethylpyridine (3.3 g) was obtained by distillation at 198-200 (760 mm).

With the rapid development of chemical substances, we look forward to future research findings about 7477-10-3.

Reference:
Patent; Merck & Co., Inc.; US4279913; (1981); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 1132-37-2 , The common heterocyclic compound, 1132-37-2, name is Dipyridin-2-ylmethane, molecular formula is C11H10N2, 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.

[0158] Benzyl potassium 4.0 g (30.5 mmol) was added into a solution of dipyridin-2-ylmethane 5.2 g (30.5 mmol) in 100 mL THF at -70 C. over 10 minutes. The mixture was stirred at ambient temperature for 16 hours after which the bright yellow mixture was filtrated and washed with THF. Solvents were evaporated and the product washed with pentane and evaporated to yield a bright yellow solid which on the basis of the 1H-NMR spectrum in DMSO-d6 was [DPM-K+] [THF]0.5. Yield 5.44 g (73.0%) based the THF complex (Mw=244.35 g mol-1). The product decomposed during ETMS analysis. Elemental analysis calculated for [DPM-K+] [THF]0.5: C 64.6%, H 4.8%, N 12.0%, K 21.9%. Found: C 63.9%, H 5.36%, N 11.46%, K 16.0%. NMR spectra were recorded at +22.7 C., +50 C. and at +70 C. in DMSO-d6. The complex shows fluxional behaviour in NMR with increasing temperature which is caused by the transition between the two resonance structures A and B. The peaks coalescence at +70 C. The singlet bridgehead proton is exchanged slowly with the methyl deuterium of DMSO-d6 which is seen as an appearing triplet in 13C-NMR. 1H-NMR in DMSO-d6 at +70 C. delta: 8.20 and 6.25 (broad coalesence peaks, 2H, from HaHa’), 7.65 (d, 2H, from HdHd’), 6.78 (broad, 2H, from HbHb’), 5.76 (broad, 2H, from HcHc’), 4.62 (S, 1H, exchangeable proton He). 13C-NMR in DMSO-d6 at delta: 160.2, 147.9, 147.8, 132.3, 131.2, 116.9, 114,3, 105.3, 103.3, triplet 87.2 from exchanged CHeDMSO-d6. 13C-CPMAS delta: 163, 150, 138, 119, 109, 82.

The synthetic route of 1132-37-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Andell, Ove; Maaranen, Janne; Hoikka, Jouni; Vanne, Tiina; Rautio, Soile; US2003/225275; (2003); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 6318-51-0, 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. 6318-51-0, name is (4-Chlorophenyl)(pyridin-2-yl)methanone. A new synthetic method of this compound is introduced below.

0.2 g of (4-chlorophenyl) (2-pyridyl) methanone was dissolved in 2 mL of hydrogen peroxide (mass concentration of 30% aqueous solution) 1.0 mL of acetic acid was added and the reaction was heated to 85 C. for 12 h. The progress of the reaction was monitored by TLC until the reaction was complete. The mixture was saturated with sodium bicarbonate, extracted with dichloromethane, washed, and the organic phases were combined, dried over anhydrous sodium sulfate, filtered, Removal of the solvent gave 0.21 g of a white solid in 95% yield.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,6318-51-0, (4-Chlorophenyl)(pyridin-2-yl)methanone, and friends who are interested can also refer to it.

Reference:
Patent; Yichang Renfu Pharmaceutical Co., Ltd.; China Three Gorges University; Fu Yigang; Lv Jinliang; Zhou Haifeng; Wang Baigui; Cao Lu; Zheng Huazhang; Tian Luanyuan; Li Shiqun; Li Lie; Du Wentao; (13 pag.)CN106938995; (2017); 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. 6960-22-1, name is 6-Methylnicotinamide. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 6-Methylnicotinamide

Example 4: Synthesis of 106Step 1 :3.00 g (22.0 mmol) 6-methylnicotinamide is dissolved in 10 ml THF under argon-atmosphere and 34 ml (34 mmol; 1.5 eq.) 1 M lithium aluminum hydride in THF are added. After 45 min additional lithium aluminum hydride (1.22 g; 1.5 eq.) in 40 ml THF is added. The reaction mixture is heated to 60C for 24 h under stirring. The reaction mixture is carefully quenched under stirring with isopropyl alcohol, methanol and finally water at 0C. The solvent is removed under vacuum. After addition of 100 ml 2N NaOH solution and 100 ml DCM the white precipitate is centrifuged off and the aqueous layer is extracted 4 times with 60 ml DCM. The combined organic layers are dried over magnesium sulphate and the solvent is removed under reduced pressure yielding 1.57 g (12.9 mmol; 58%) of the amine 2 which is used without further purification for subsequent reaction steps.

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, 6960-22-1, 6-Methylnicotinamide.

Reference:
Patent; JERINI AG; WO2006/128670; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 72648-12-5, 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.72648-12-5, name is 2-Chloro-3-(trichloromethyl)pyridine, molecular formula is C6H3Cl4N, molecular weight is 230.91, as common compound, the synthetic route is as follows.

The 2-chloro-3-trichloromethylpyridine is hydrolyzed to obtain a 2-chloronicotinic acid reaction product, and the reaction formula is as follows

Statistics shows that 72648-12-5 is playing an increasingly important role. we look forward to future research findings about 2-Chloro-3-(trichloromethyl)pyridine.

Reference:
Patent; Weifang Xinlv Chemical Co., Ltd.; Han Zengrui; Sun Zaichen; Han Zhiren; Zhang Jinwang; Jiang Dongsheng; (10 pag.)CN110229098; (2019); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem