Day: March 25, 2022

Synthetic Route of 1137-67-3, 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. 1137-67-3, name is 2-(Pyridin-3-yl)-1H-benzo[d]imidazole, molecular formula is C12H9N3, 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.

General procedure: A solution of 2-(3-pyridyl)-1H-benzimidazole, L1, (0.34 g,1.79 mmol) in methanol (4 ml) was added to a solution ofZn(OAc)22H2O (0.39 g, 1.79 mmol) in methanol (6 ml).The mixture was stirred for 24 h at room temperature to give a white precipitate. After the reaction period, the precipitate was filtered off, washed with methanol (3 9 20 mL) and dried to afford complex 1 as a white solid.

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 1137-67-3, 2-(Pyridin-3-yl)-1H-benzo[d]imidazole.

Reference:
Article; Zaca, Thembisile P.; Ojwach, Stephen O.; Akerman, Matthew P.; Transition Metal Chemistry; vol. 41; 6; (2016); p. 663 – 673;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 160590-36-3, 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. 160590-36-3, name is 2-Methoxy-3-nitro-4-methylpyridine. A new synthetic method of this compound is introduced below.

Sodium acetate (365 g, 5.37 mol) was added to a stirred solution of 2-methoxy-4-methyl-3-nitropyridine (250 g, 1.49 mol) in acetic acid (1 .5 L) at ambient temperature and then Br2(639 g, 4.00 mol) was added dropwise (30 mm). After addition, the mixture was heated at 80C for 12 h, at which time TLC indicated the reaction had gone to completion. The mixturewas cooled (0 C) and quenched by sequential addition of 10% aqueous (1.5 L) and saturatedaqueous sodium sulfate (1.5 L). The resulting solid was collected by filtration, washed withwater, and dried under reduced pressure to give the title compound (302 g, 82.2% yield) as alight yellow solid. h11 NMR (400 MHz, DMSO-d6): 6 8.25 (s, 1 H), 3.94 (s, 3 H), 2.29 (s, 3H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,160590-36-3, 2-Methoxy-3-nitro-4-methylpyridine, and friends who are interested can also refer to it.

Reference:
Patent; GENENTECH, INC.; CONSTELLATION PHARMACEUTICALS, INC.; ALBRECHT, Brian, K.; BELLON, Steven, F.; BURDICK, Daniel, J.; COTE, Alexandre; CRAWFORD, Terry; DAKIN, Les, A.; HEWITT, Michael, Charles; HSIAO-WEI TSUI, Vickie; LEBLANC, Yves; MAGNUSON, Steven, R.; NASVESCHUK, Christopher, G.; ROMERO, F., Anthony; TANG, Yong; TAYLOR, Alexander, M.; WANG, Shumei; (197 pag.)WO2016/77378; (2016); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 33252-29-8 ,Some common heterocyclic compound, 33252-29-8, molecular formula is C6H3ClN2, 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.

General procedure: In a 1L four-necked flask equipped with a mechanical stirring and condensation device,Put in homemade 2-chloro 6-cyanopyridine (calculated as pure product,The same below) 600g, tungsten hexachloride 12g, phosphorus pentachloride 12g, atmospheric pressure,Heat up to 150 , start stirring, and continuously introduce chlorine gas at a rate of 100mL/min.Control the reaction temperature at 150 ~ 155 , continuous reaction for 20h,Sampling gas chromatography analysis, raw material conversion rate and product yield are shown in Table 2.

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. 33252-29-8, 6-Chloropicolinonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nanjing Hong Sun Biochemical Co., Ltd.; Chen Honglong; Mu Dengyou; Wang Fujun; Jiang Jianhua; Xue Yi; Chen Xinchun; (7 pag.)CN111072558; (2020); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 15862-50-7, 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 15862-50-7 as follows.

Dioxane (10.4 L, 8 v), 1 (1.3 kg, 1.0 eq.), KOAc (1.65 kg, 3.0 eq.), and B2Pin2 (1.7 kg, 1.2 eq.) were charged into 20 L reactor. Nitrogen was bubbled into the solution to remove any excess oxygen for 1 hour at 20~30C. Pd(dppf)Cl2 (125.6 g, 0.03 eq.) was into the reactor into the mixture under nitrogen. The mixture was heated to 80~90C. Thehe reaction mixture stirred for 3 hours at until HPLC showed the reaction was completed. The reaction mixtiire was cooled to 20-30C and then filtered. The filtered cake was washed with dioxane (2.6 L, 2 v). The filtered solutions were combined and concentrated and then transferred to 20 L reactor. H2O2 (3.25 L, 2.5 v) was added at 20~50C, and the temperature was increased from 23 to 50C. The reaction misture was stirred for 30-60 min until HPLC showed the reaction was completed. H2O (6.5 L, 5 v) was added in to the mixture, and the mixture was extracted with DCM (13.0 L, 10 v) twice. The organic phase was collected and washed with 15% brine (6.5 L, 5 v) twice, and was then extracted with 15% Na2C03 (6.5 L, 5 L) twice. The aqueous phase was colleted and the pH value was ajdjusted 10-1 1 to 4-5 with 3M HC1. The aqueous phase was then extracted with EA (13.0 L, 10.0 v) twice. The organic phase was collected and concentrated to about dryness, and heptane (6.5 L, 5.0 v) was added to slurry for 1 hour at 20~30C. The slurry was filtered, and the filtered cake was washed with heptane (650 ml, 0.5 v), drid in oven at 30~40C for overnight to obtain 650.2 g product as brown solid with purity: 99.6%, yield: 67.8%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,15862-50-7, its application will become more common.

Reference:
Patent; EPIZYME, INC.; CAMPBELL, John Emmerson; DUNCAN, Kenneth William; MILLS, James Edward John; MUNCHHOF, Michael John; (301 pag.)WO2019/79540; (2019); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 1042141-37-6, 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 1042141-37-6, name is Methyl 2-bromoimidazo[1,2-a]pyridine-6-carboxylate. This compound has unique chemical properties. The synthetic route is as follows.

Methyl 2-bromoimidazo[1,2-ajpyridine-6-carboxylate (300 mg, 1.18 mmol) dissolved in diethyl ether (12 mL) and cooled to 0 C was treated with lithium aluminum hydride (46 mg, 1.21 mmol). The reaction mixture was allowed to warm to room temperature and stirred overnight. Aftercooling to 0 C again, the reaction mixture was quenched by addition of sodium sulfate decahydrate. The mixture was stirred for 20 mm and filtered. The filtrate was concentrated to give (2-bromoimidazo[1,2- ajpyridin-6-yl)methanol.

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 1042141-37-6, Methyl 2-bromoimidazo[1,2-a]pyridine-6-carboxylate.

Reference:
Patent; GILEAD SCIENCES, INC.; AKTOUDIANAKIS, Evangelos; APPLEBY, Todd; CHO, Aesop; DU, Zhimin; GRAUPE, Michael; GUERRERO, Juan A.; JABRI, Salman Y.; LAD, Lateshkumar Thakorlal; MACHICAO TELLO, Paulo A.; MEDLEY, Jonathan William; METOBO, Samuel E.; MUKHERJEE, Prasenjit Kumar; NADUTHAMBI, Devan; NOTTE, Gregory; PARKHILL, Eric Q.; PHILLIPS, Barton W.; SIMONOVICH, Scott Preston; SQUIRES, Neil H.; VENKATARAMANI, Chandrasekar; WANG, Peiyuan; WATKINS, William J.; XU, Jie; YANG, Kin Shing; ZIEBENHAUS, Christopher Allen; (724 pag.)WO2018/195321; (2018); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 52605-96-6 ,Some common heterocyclic compound, 52605-96-6, molecular formula is C6H6ClNO, 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, 3-Dimethoxypyridine (40) To a stirring solution of sodium methoxide (300.0 mL, 30% in methanol) was added 2-chloro-3-methoxypyridine (55.0 g, 383.1 mmol). The reaction mixture was stirred at 80 C. overnight. After the reaction was completed, the mixture was evaporated in vacuo. The residue was dissolved with ethyl acetate, washed with brine, dried over anhydrous sodium sulfate and filtered. The filtrate was evaporated in vacuo. The residue was purified by flash chromatogram with ethyl acetate/petroleum ether (1:5) to afford 2,3-dimethoxypyridine (40) as yellow oil (42.0 g, 79%). ESI-MS, m/z=140 [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. 52605-96-6, 2-Chloro-3-methoxypyridine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Tsai, Guochuan Emil; Wang, Ching-Cheng; Hsieh, Yuan-Ting; (53 pag.)US2019/112289; (2019); A1;,
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. 2897-43-0, name is 2,6-Dichloro-3-nitropyridin-4-amine, molecular formula is C5H3Cl2N3O2, 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. name: 2,6-Dichloro-3-nitropyridin-4-amine

Intermediate 3: 2,6-Dichloro-3,4-pyridinediamine 2,6-dichloro-3-nitro-4-pyridinamine (881 mg, 4.24 mmol) was taken up in ethanol (15 ml) and tin(II) chloride (3212 mg, 16.94 mmol) was added portion wise over 5 min. The resulting pale yellow solution was allowed to stir at 50 C. under N2 for 3 h, LCMS showed approx 60% conversion, the reaction was left for a further 3 h, LCMS showed almost complete conversion. The reaction was allowed to cool to room temperature and was partitioned between NaHCO3 (aq) (50 ml) and EtOAc (50 ml). The organic layer was dried using a hydrophobic frit, concentrated and dried in vacuo overnight to give the title compound as a yellow solid (734 mg). LCMS (Method B): Rt=0.57 min, MH+=178

With the rapid development of chemical substances, we look forward to future research findings about 2897-43-0.

Reference:
Patent; GLAXO GROUP LIMITED; Atkinson, Francis Louis; Atkinson, Stephen John; Barker, Michael David; Douault, Clement; Garton, Neil Stuart; Liddle, John; Patel, Vipulkumar Kantibhai; Preston, Alexander G.; Shipley, Tracy Jane; Wilson, David Matthew; Watson, Robert J.; US2014/5188; (2014); 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 58602-02-1, name is 2,6-Difluoro-3-nitropyridine. This compound has unique chemical properties. The synthetic route is as follows. Computed Properties of C5H2F2N2O2

STEP B: 6-Fluoro-2-(3,4-methylenedioxyanilino)-3-nitropyridine In 75 ml. of ethanol was dissolved 3.2 g. (0.002 mole) of 2,6-difluoro-3-nitropyridine followed by 1.68 g. (0.02 mole) of sodium bicarbonate. To this stirred mixture, was added a solution of 2.74 g. (0.02 mole) of 3,4-(methylenedioxy) aniline in 50 ml. of ethanol dropwise over 45 minutes at room temperature. After one hour, 100 ml. of water was added and the deep-red crystalline solid product was collected. A small amount was crystallized from ethanol and melted at 161-162 C.

With the rapid development of chemical substances, we look forward to future research findings about 58602-02-1.

Reference:
Patent; Merck & Co., Inc.; US4144341; (1979); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 868551-30-8 ,Some common heterocyclic compound, 868551-30-8, molecular formula is C8H8N2O4, 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.

A mixture of methyl 4- methyl-5-nitropyridine-2-carboxylate (3.5g, 17.8mmol), dimethylformamide dimethylacetal (DMF- DMA) (3.6ml, 1.5eq) in acetonitrile (35mL) was heated in a microwave at 14O0C for 20 min. The solvent was removed. The residue (5.1 g) was carried onto the next step without further purification. Method 2. A mixture of compound methyl 4-methyl-5-nitropyridine-2-carboxylate (39.5g, 0.19mol), DMF-DMA (30.6 g, 0.26mol, 1.35 eq) in DMF (470 mL) was heated to 90C for 30 min. The solvent was removed in vacuo. The residue (78g) was used without further purification in the next step.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,868551-30-8, its application will become more common.

Reference:
Patent; PFIZER INC.; WO2006/27694; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 22353-40-8, Adding some certain compound to certain chemical reactions, such as: 22353-40-8, name is 2,3-Dichloro-5-nitropyridine,molecular formula is C5H2Cl2N2O2, 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 22353-40-8.

EXAMPLE 10 3-amino-5,6-dichloropyridine 77.2 g (0.4 mol) of 2,3-dichloro-5-nitropyridine were dissolved in 135 ml of glacial acetic acid, and 800 ml of water were added with stirring. 111.7 g (2 mol) of iron powder were introduced in portions into the mixture (temperature?50 C.). After completion of the reaction, the mixture is filtered under suction and the product extracted using ethyl acetate. The organic phase was washed with water until neutral, dried using MgSO4 and concentrated by evaporation. The product was recrystallized from toluene. Yield 85% Melting point 107 C.

According to the analysis of related databases, 22353-40-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Hoechst Aktiengesellschaft; US4756739; (1988); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem