Day: April 7, 2022

Reference of 53636-70-7, 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 53636-70-7 as follows.

In a 100 ml round-bottomed flask 6-methyl-2,3-pyridinedicarboxylic acid (10 g, 55.2 mmol) and acetic anhydride (26 ml, 276 mmol) were added and heated at 100 C under nitrogen for 5 hours. After this time the volatiles were removed under vacuum to give the title compound D60 (8.2 g) as a slightly brown solid. 1H NMR (400 MHz, DMSO-d6) delta ppm 8.41 (d, 1 H), 7.82 (d, 1 H), 2.73 (s, 3 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,53636-70-7, its application will become more common.

Reference:
Patent; GLAXO GROUP LIMITED; DI FABIO, Romano; WO2012/89607; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 685115-77-9, 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 685115-77-9 as follows.

To a solution of 1-(3,5-dichloropyridin-4-yl)piperidine-4-carboxamide 23 (0.10 g, 0.36 mmol) in polyphosphoric acid (5 ml.) at 80 0C was added vinylene carbonate (35 mg,0.40 mmol). The mixture was heated at 170 0C for 4 hours, cooled to r.t. and poured into water (200 ml_). The mixture was extracted with ethyl acetate (3 x 50 ml.) and the combined organic extracts were washed with water (100 ml_), a saturated solution of sodium hydrogen carbonate (50 ml_), water (50 ml_), brine (50 ml_), dried (MgSO4) and concentrated under reduced pressure to furnish a colourless oil (12 mg). The crude product was purified by preparative tic on silica gel (CH2CI2, MeOH, 10:1 then hexane,EtOAc, 1 :1 ) to furnish the title compound as a white solid (13 mg, 12%), LC-MS (ESI) Rt 2.66 min, m/z 298 (100%, M+); m/z (ESI) Ci3H14CI2N3O requires 298.0508 found [M+H]+ 298.0507.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,685115-77-9, its application will become more common.

Reference:
Patent; CANCER RESEARCH TECHNOLOGY LIMITED; McDONALD, Edward; BLAGG, Julian; PICHOWICZ, Mark; CRUMPLER, Simon Ross; WO2010/41054; (2010); 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. 670253-37-9, name is 4-Chloro-5-iodopyridin-2-amine, the common compound, a new synthetic route is introduced below. Application In Synthesis of 4-Chloro-5-iodopyridin-2-amine

A mixture of 4-chloro-5-iodopyridin-2-amine (2.8 g, 1 1 mmol), Pd(PPh3)4 (1.9 g, 1.65 mmol), and Zn(CN)2 (0.7 g, 6.05 mmol) in NMP (30 mL) was heated at 130C for 5 hours. The reaction mixture was cooled to 23C, diluted by H20 (200 mL) and filtered. The solid was purified by silica gel chromatography using Petroleum Ether:EtOAc (3: 1 ) as eluting solvents to afford 2-(3H- imidazo[4,5-b]pyridin-3-yl)acetimidamide as a yellow solid (1.18 g, 70%). MS (ESI) m/z: 154 [M+H]+.

The synthetic route of 670253-37-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BEAUFOUR IPSEN TIANJIN PHARMACEUTICAL CO., LTD; AUVIN, Serge; LAVERGNE, Olivier; CHAO, Qi; CHEN, Yufeng; WO2015/100609; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Application of 91678-23-8, Adding some certain compound to certain chemical reactions, such as: 91678-23-8, name is 2-Bromo-6-chloro-3-nitropyridine,molecular formula is C5H2BrClN2O2, 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 91678-23-8.

Under nitrogen a solution of 2-bromo-6-chloro-3-nitropyridine (2.5 g, 10.53 mmol, 1.00 equiv) in THF (60 mL) was cooled to -78 C. and bromo(ethenyl)magnesium (1M in THF, 63 mL, 6 equiv) was added dropwise. The reaction was stirred for 1 h at -50 C., quenched with aqueous ammonium chloride, extracted with ethyl acetate, dried over sodium sulfate, and concentrated in vacuum. The residue was purified by silica gel column chromatography eluting with ethyl acetate/petroleum ether (1:3). This resulted in the title compound (1.3 g, 53%) as a yellow solid. LC-MS (ES, m/z): 231 [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. 91678-23-8, 2-Bromo-6-chloro-3-nitropyridine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Genentech, Inc.; Blaquiere, Nicole; Castanedo, Georgette; Feng, Jianwen A.; Hu, Baihua; Staben, Steven; Yuen, Po-wai; Wu, Guosheng; Lin, Xingyu; Burch, Jason; US2015/57260; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 274-76-0 ,Some common heterocyclic compound, 274-76-0, molecular formula is C7H6N2, 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 DMF (120 mL, 1.55 mol) at 2 C, freshly distilled phosphorus oxychloride (61 mL, 0.65 mol) was slowly added. The temperature was allowed to rise gradually to room temperature. The solution was cooled again to 2 C and a solution of imidazo[1,2-a]-pyridine 1 (10 g, 0.085 mol) in DMF (60 mL) was added dropwise. The mixture was warmed to 105 C, whereupon the temperature rose to 140 C. The oil bath was removed until the temperature stabilized at 120 C. The reaction mixture was heated for 45 min at 120 C and 2.5 h at 85 C, then cooled and poured into 5% HCl (600 mL) ice-cooled and brought to pH 9 using 20% NaOH. The resulting solution was extracted with CH2Cl2 (1200 mL) overnight. Then the organic layer was separated and dried over MgSO4, the solvent removed under reduced pressure, the crude product washed with water (5 × 15 mL) and again dried, providing the pure product 3.49 g (31%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,274-76-0, its application will become more common.

Reference:
Article; B?aewska, Katarzyna M.; Ni, Feng; Haiges, Ralf; Kashemirov, Boris A.; Coxon, Fraser P.; Stewart, Charlotte A.; Baron, Rudi; Rogers, Michael J.; Seabra, Miguel C.; Ebetino, Frank H.; McKenna, Charles E.; European Journal of Medicinal Chemistry; vol. 46; 10; (2011); p. 4820 – 4826;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 1235036-15-3, 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 1235036-15-3, name is tert-Butyl 3-bromo-6-chloropicolinate. This compound has unique chemical properties. The synthetic route is as follows.

To a solution of tert-butyl 3-bromo-6-chloropicolinate (5.92 g) in tetrahydrofuran (60 mL) and water (30 mL) was added the crude Example 1.20.1 (4.44 g), 1,3,5,7-tetramethyl-6-phenyl-2,4,8-trioxa-6-phosphaadamante (1.5 g), tris(dibenzylideneacetone)dipalladium(0) (927 mg) and K3PO4(22 g). the mixture was stirred at reflux overnight, cooled, diluted with ethyl acetate (800 mL) and washed with water and brine. The organic layer was dried over sodium sulfate, filtered, and concentrated. residue was purified by flash chromatography, eluting with 20% ethyl acetate in heptane followed by 5% methanol in dichloromethane, to give the title compound. MS (ESI) m/e 531.1 (M+H)+.

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 1235036-15-3, tert-Butyl 3-bromo-6-chloropicolinate.

Reference:
Patent; AbbVie Inc.; Benatuil, Lorenzo; Bruncko, Milan; Chao, Debra; Izeradjene, Kamel; Judd, Andrew S.; Phillips, Andrew C.; Souers, Andrew J.; Thakur, Archana; (556 pag.)US2017/355769; (2017); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 1256823-07-0, 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 1256823-07-0, name is 5-Bromo-4-methoxypicolinonitrile. This compound has unique chemical properties. The synthetic route is as follows.

Synthesis of 4-methoxy-5-(4-methyl-lH-imidazol-l-yl) picolino nitrile [0324] To a stirred solution of 4-methyl-lH-imidazole (580 mg, 7.04 mmol) in acetonitrile (24 mL) under argon atmosphere were added potassium carbonate (1.3 g, 9.38 mmol) and 18 crown-6 (2.47 g, 9.38 mmol) at RT. The reaction mixture was stirred at 60 C for 2 h. Then 5-bromo-4-methoxypicolinonitrile (1 g, 4.69 mmol) was added to the reaction mixture and stirred at reflux for 18 h. After consumption of the starting materials (monitored by TLC), the reaction was diluted with water (20 mL) and extracted with EtOAc (2 x 30 mL). The combined organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo. The crude material was purified by silica gel column chromatography using 90%> EtOAc:hexanes to afford 4-methoxy-5-(4-methyl-lH-imidazol-l-yl) picolino nitrile (250 mg, 25%) as a yellow solid. 1H-NMR (CDC13, 500 MHz): delta 8.58 (s, 1H), 7.82 (s, 1H), 7.39 (s, 1H), 6.99 (s, 1H), 401 (s, 3H), 2.23 (s, 3H); LC-MS: 215 (M+l); (column; X-Bridge C-18 (50 3.0 mm, 3.5 mu); RT 2.45 min. 0.05% Aq TFA: ACN; 0.8 mL/min); TLC: EtOAc (R 0.2).

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 1256823-07-0, 5-Bromo-4-methoxypicolinonitrile.

Reference:
Patent; FORUM PHARMACEUTICALS INC.; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; MCRINER, Andrew, J.; WO2015/66697; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 1254473-66-9, 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. 1254473-66-9, name is 1-(3,5-Dichloropyridin-4-yl)ethanol, molecular formula is C7H7Cl2NO, 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.

Separate the mixture of stereoisomers obtained in Preparation 1 on a CHIRALPAK AD-H column eluting with 90% heptanes/10% ethanol. Peak 2 is the desired enantiomer. To establish the absolute configuration dissolve a sample of the product in CDCl3 (final concentration 100 mg/mL). Obtain the vibrational circular dichroism (VCD) and infra red (IR) spectra with a resolution of 4 cm-1 using a ChiralIR FT VCD spectrometer (BioTools Inc) with an IR cell equipped with BaF2 windows and a path length of 100 mm. Collect the VCD and IR for 6 hours with 150 muL of the sample. Present the data without smoothing or further data processing. Obtain vibrational frequencies and absorption and VCD intensities by optimizing the lowest energy conformer by Gaussian at the B3PW91/6-31G** level on a Linux cluster, and simulate the corresponding spectra using a Lorentzian bandwidth of 6 cm-1 vibrational circular dichroism. The above analysis shows the product to be the S-isomer. Yield: 84.37 g (27%). MS (ES) m/z 192 [M+1]+.

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 1254473-66-9, 1-(3,5-Dichloropyridin-4-yl)ethanol.

Reference:
Patent; ELI LILLY AND COMPANY; US2012/83511; (2012); 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. 182924-36-3, name is 5-(Bromomethyl)-2-chloropyridine, the common compound, a new synthetic route is introduced below. COA of Formula: C6H5BrClN

To a solution of 323 mg (1.10 mmol) of (2-AMINO-5-PROPARGYLOXY-PHENYL)-4- isopropyl-phenyl) -methanone and 250 mg (1.21 mmol) of 2-bromomethyl-2-chloro- pyridine (step A) in 2 ml 1, 3-dimethyl-2-imidazolidinone (DMEU) 213 mg (1.54 mmol) of potassium carbonate are added. The reaction is complete after stirring for 2 h at 60 C. The cooled yellow suspension is distributed between ethyl acetate and bicarbonate solution. Flash chromatography (hexane/ethyl acetate) affords a yellow solid. m. p. 96 C. ‘H-NMR (300 MHz, CDC13) : 8.49 (t, 1H), 8.40 (d, 1H), 7.67 (dd, 1H), 7.61 (d, 2H), 7.31 (d, 2H), 7.30 (d, 1H), 7.23 (d, 1H), 7.08 (dd, 1H), 6.59 (d, 1H), 4.53 (d, 2H), 4.48 (d, 2H), 2.99 (HEPT, 1H), 2.48 (t, 1H), 1.31 (d, 6H). MS: 419 (M+L)

The synthetic route of 182924-36-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2004/56365; (2004); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 597532-36-0, 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. 597532-36-0, name is Ethyl 6-(trifluoromethyl)nicotinate. A new synthetic method of this compound is introduced below.

A mixture of ethyl 6-(trifluoromethyl)nicotinate (2.2 g, 10 mmol), Pd/C (10 wt.%, 100 mg) and platinum(IV)oxide (150 mg, 0.661 mmol) in acetic acid (30 mL) was stirred in a steel bomb under hydrogen atmosphere (200 psi) at 25 C for 24 hrs. The reaction mixture was filtered through a pad of celite and washed with MeOH (150 mL). The filtrate was concentrated under reduced pressure providing crude ethyl 6-(trifluoromethyl)piperidine-3- carboxylate (776 mg; mixture of cis and trans isomers) as a colorless oil, which was directly used in the next step without further purification. LCMS (m/z): 226.1 [M+H]+; Rt = 0.36 min.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,597532-36-0, Ethyl 6-(trifluoromethyl)nicotinate, and friends who are interested can also refer to it.

Reference:
Patent; NOVARTIS AG; BARSANTI, Paul, A.; HU, Cheng; JIN, Xianming; NG, Simon, C.; PFISTER, Keith, B.; SENDZIK, Martin; SUTTON, James; WO2012/101064; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem