Day: April 19, 2022

Reference of 1254473-66-9, 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.1254473-66-9, name is 1-(3,5-Dichloropyridin-4-yl)ethanol, molecular formula is C7H7Cl2NO, molecular weight is 192.04, as common compound, the synthetic route is as follows.

S)- 1 -(3,5-Dichloropyridin-4-yl)ethanol Separate the mixture of stereoisomers obtained in the above reaction 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 CDCI3 (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 B3PW91/6-3 IG** 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 [MH-I]+.

The chemical industry reduces the impact on the environment during synthesis 1254473-66-9, I believe this compound will play a more active role in future production and life.

Reference:
Patent; ELI LILLY AND COMPANY; CHEN, Daohong; LI, Hong-Yu; ZHAO, Genshi; WO2010/129509; (2010); 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. 1196152-34-7, name is 2-Bromo-6-methoxypyridin-4-amine, molecular formula is C6H7BrN2O, 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. COA of Formula: C6H7BrN2O

In a 50 mL single collar flask 500 mg (2.4 mmol, 1 eq) of 2 bromo-6-methoxy-pyridin-4- ylamine were introduced, to which was added 20 mL of toluene and 586 mg (4.92 mmol, 2 eq) of thionyl chloride, and the mixture heated at reflux for 3 hours. The reaction medium was dry concentrated under vacuum, and the residue was returned to solution in 20 mL of acetonitrile. 325 mg (2.46 mmol, 1 eq) of 2-hydroxy-2-methyl-pentanoic acid was then added at ambient temperature. After 16 hours at ambient temperature, the reaction mixture was heated to 80C for 4 hours, then to 60C for 3 days, and the reaction mixture was then dry concentrated. The residue was dissolved in 50 mL ethyl acetate. The solution was washed twice with 50 mL of an aqueous solution saturated with ammonium chloride, and then twice with 50 mL of water. The organic phase was then dried over magnesium sulphate and then dry concentrated under vacuum. A brown oil was obtained which was purified by chromatography on silica with a 1/1 (v/v)heptane/ethyl acetate mixture as the eluent. A brown solid was then obtained and purified by chromatography on grafted C18 silica with a water / acetonitrile mixture as the eluent (gradient 5 at 100% acetonitrile). 2-Hydroxy-2-methyl-pentanoic acid (2-bromo-6- methoxy-pyridin-4-yl)-amide was obtained in the form of a white solid. Melting point = 122C. NMR (1H, DMSO): 0.9 (t; 3H; J=4 Hz); 1.1 -1.3 (m; 1 H); 1.4 (s; 3H); 1.4-1 .5 (m; 1 H); 1.6 (m; 1 H); 1 .7 (m; 1 H); 3.9 (s; 3H); 5.8 (s; 1 H); 7.4 (d; 1 H; J=1 .4 Hz); 7.8 (d; 1 H; J=1 .4 Hz); 10.2 (s; 1 H).

With the rapid development of chemical substances, we look forward to future research findings about 1196152-34-7.

Reference:
Patent; GALDERMA RESEARCH & DEVELOPMENT; POINSARD, Cedric; WO2013/64681; (2013); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 717843-56-6, 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 717843-56-6, name is 3-Bromo-2-methoxy-5-methylpyridine. This compound has unique chemical properties. The synthetic route is as follows.

Step 2: 3-Bromo-2-methoxy-5-methyl-pyridine (4.0 g, 19.8 mmol), N-bromosuccinimide (4.45 g, 23.8 mmol), and azobisisobutyronitrile (0.163 g, 0.99 mmol) were combined in benzene (40 mL) and stirred overnight at 80 C. The reaction was stirred for another 24 hours at 80 C., and then additional N-bromosuccinimide (1.8 g, 10.1 mmol), and azobisisobutyronitrile (catalytic) were added. After stirring for another 2 hours at 80 C., the mixture was diluted with H2O and extracted with CH2Cl2. The residue was purified by silica gel chromatography to give 3-bromo-5-bromomethyl-2-methoxy-pyridine.

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 717843-56-6, 3-Bromo-2-methoxy-5-methylpyridine.

Reference:
Patent; AMIRA PHARMACEUTICALS, INC.; US2010/81673; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 64690-19-3 ,Some common heterocyclic compound, 64690-19-3, molecular formula is C13H22N2, 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. A mixture of 4-octylaminopyridine (10 g., 0.048 mole) and octyl bromide (8 ml., 0.048 mole) was heated at 125 C. for 8 hr. on one day and for 4 more hr. on the next day. The resulting solid was slurried, first in ether, then in ether-tetrahydrofuran (2:1) and finally in tetrahydrofuran, collected by filtration, washed with ether on the filter, and dried (70 C., 0.1 mm.) affording N-(1-octyl-4(1H)-pyridinylidene)octanamine monohydrobromide (11.95 g., 83% yield, m.r. 108-112 C.), which is the monohydrobromide salt of the compound of Formula I wherein both R and R’ are octyl.

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. 64690-19-3, 4-(Octylamino)pyridine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sterling Drug Inc.; US4598082; (1986); A;; ; Patent; Sterling Drug Inc.; US4839372; (1989); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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. 1033203-41-6, name is 6-Bromopyridine-3,4-diamine. A new synthetic method of this compound is introduced below., COA of Formula: C5H6BrN3

6-Bromopyridine-3,4-diamine (200.0 mg, 1.06 mmol) was added to diethyl oxalate (3.0 mL). The mixture was stirred at 130 C. for 12 hours and then cooled to room temperature. Et2O was added thereto to form a solid. The formed solid was filtered and dried under reduced pressure to obtain brown solid compound of 7-bromopyrido[3,4-b]pyrazine-2,3-diol (195.0 mg, 76%). [1236] 1H-NMR (400 MHz, DMSO-d6); delta: 12.23 (brs, 1H), 12.11 (brs, 1H), 8.09 (s, 1H), 7.05 (s, 1H)

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, 1033203-41-6, 6-Bromopyridine-3,4-diamine.

Reference:
Patent; C&C RESEARCH LABORATORIES; Ho, Pil Su; Yoon, Dong Oh; Han, Sun Young; Lee, Won Il; Kim, Jung Sook; Park, Woul Seong; Ahn, Sung Oh; Kim, Hye Jung; US2014/315888; (2014); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 108118-69-0, 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 108118-69-0 as follows.

To a suspension of l-methyl-lH-pyrrolo[2,3-b]pyridine-5-carboxylic acid (3.54 g, 20.1 mmol) in CH2Cl2 (400 mL) was added l-chloro-N,N-2-trimethylpropenylamine (5.26 mL, 40.2 mmol). Following formation of the resulting acid chloride, the reaction mixture was concentrated affording a residue that was dissolved in pyridine (100 mL) before 2,6- difluoro-pyridin-3-ylamine (2.61 mg, 20.1 mmol) was added in one portion. After an additional 30 minutes the reaction mixture was concentrated to dryness affording a residue, to which was added water causing precipitation o f analytically pure 1 -methyl- 1 H-pyrrolo [2,3 -»]pyridine- 5 – carboxylic acid (2J6-difluoro-pyridin-3-yl)-amide (4.2 g, 72.5% yield). ES MS (M+H+) = 289

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,108118-69-0, its application will become more common.

Reference:
Patent; MERCK & CO., INC.; WO2009/155017; (2009); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 6854-07-5, 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. 6854-07-5, name is 5-Nitro-2-oxo-3-pyridinecarboxylic Acid, molecular formula is C6H4N2O5, 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.

b) 2-Chloro-5-nitro-nicotinic acid 2-Hydroxy-5-nitro-nicotinic acid (2.7 mmol) in a mixture of NJV- dimethylformamide (2.7 mmol) and thionyl chloride (5 ml) was heated at 80 0C for 1 h. The mixture was allowed to cool and concentrated in vacuo. To the resulting residue was added ice-water (20 ml) and with vigorous stirring a precipitate formed. The precipitate was filtered off and dried in a vacuum oven to give a white solid (68%).ESIMS: M-I: found 201 ; expected 201; and1H NMR (300 MHz, DMSO) ? 9.30 (IH, d, H-4), 8.83 (IH, d, H-6).

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 6854-07-5, 5-Nitro-2-oxo-3-pyridinecarboxylic Acid.

Reference:
Patent; BIONOMICS LIMITED; WO2008/46135; (2008); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 98121-41-6, 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 98121-41-6, name is 3-Amino-5,6-dichloropyridine. This compound has unique chemical properties. The synthetic route is as follows.

A 5L flask with mechanical stirrer, thermocouple, and addition funnel was charged with the product of Example 2C (70 g, 429 mmol) and 48% HBraq (240 mL). The suspension was maintained at 0-5 C. as a solution of NaNO2 (32.0g, 464 mmol) in water (100 mL) was added dropwise over 1 hour. Additional water (200 mL) was added and the mixture was stirred for 10 minutes at 0-5 C. The mixture was treated with CuBr (32.6 g, 227 mmol) in portions over 20 minutes followed by additional water to maintain a fluid reaction mixture. The mixture was allowed to warm to room temperature and diluted with water. The mixture was distilled at ambient pressure, until the distillate ran clear (1.5 L collected). The distillate was extracted with EtOAc (3*500 mL) and the combined extracts were washed with brine (100 mL), dried (MgSO4), and concentrated to provide 5-bromo-2,3-dichloropyridine as a solid. 1H NMR (CDCl3, 300 MHz) delta 7.94 (d, J=3 Hz, 1H), 8.38 (d, J=3 Hz, 1H).

According to the analysis of related databases, 98121-41-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Buckley, Michael J.; Ji, Jianguo; US2004/242644; (2004); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 1214328-96-7 ,Some common heterocyclic compound, 1214328-96-7, molecular formula is C7H5BrClNO2, 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 the solution of methyl 3-bromo-6-chloropyridine-2-carboxylate (5.0 g, 19.9 mmol) and MeOH (1.0 mL, 25.8 mmol) in THF (15.0 mL, freshly dried over NaH) was added /-BuOK (29.8 mL, 29.8 mmol, 1 M in THF) slowly over 20 min at 0 C under N2 atmosphere. The reaction mixture was stirred at 0 C for 5 min. The reaction mixture was quenched with ice-cold sat. NH4Cl solution (30.0 mL), and extracted with EtOAc (50.0 mL x 2) rapidly. The combined organic layers were dried over anhydrous Na2S04, filtered and concentrated. The residue was purified by flash silica gel chromatography (40 g column, EtOAc in petroleum ether from 0% ~ 10%) to give methyl-3 -bromo-6-methoxypyridine-2- carboxylate (4.5 g, 92.0% yield) as a colorless oil.

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. 1214328-96-7, Methyl 3-bromo-6-chloropicolinate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; RELAY THERAPEUTICS, INC.; D.E. SHAW RESEARCH, LLC; TAYLOR, Alexander, M.; LESCARBEAU, Andre; KELLEY, Elizabeth, H.; SHORTSLEEVES, Kelley, C.; WALTERS, W., Patrick; MURCKO, Mark, Andrew; MCLEAN, Thomas, H.; GUNAYDIN, Hakan; GIORDANETTO, Fabrizio; THERRIEN, Eric; (607 pag.)WO2019/183367; (2019); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 63572-73-6 ,Some common heterocyclic compound, 63572-73-6, molecular formula is C6H4N4O2, 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 a solution of 5-nitro-1H-pyrazolo [4,3-b]pyridine (7.3 g,38.0 mmol) in MeOH (240 mL) was added 10% wt Pd/C (4.03,3.8 mmol). The reaction mixture was hydrogenated underhydrogen (1 atm) for 16 h. The Pd/C was removed by filtration, andthe filtrate was concentrated to give 1H-pyrazolo [4,3-b]pyridin-5-amine (5.1 g, 82% yield) as a light brown solid. Rf: 0.33 (DCM/MeOH,19/1, v/v). Mp: 178 C. 1H NMR (DMSO-d6, 400 MHz) d 13.12 (s, 1H),8.05 (d, J 2.4 Hz, 1H), 7.81 (s, 1H), 7.18 (d, J 2.3 Hz, 1H), 5.04 (s,2H). MS (ESI)m/z:134.8 [MH],156.7 [MNa], 301.0 [2MNa].

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. 63572-73-6, 5-Nitro-1H-pyrazolo[3,4-b]pyridine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Hao, Chenzhou; Huang, Wanxu; Li, Xiaodong; Guo, Jing; Chen, Meng; Yan, Zizheng; Wang, Kai; Jiang, Xiaolin; Song, Shuai; Wang, Jian; Zhao, Dongmei; Li, Feng; Cheng, Maosheng; European Journal of Medicinal Chemistry; vol. 131; (2017); p. 1 – 13;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem