Day: March 18, 2021

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.80194-69-0, name is 5-(Trifluoromethyl)picolinic acid, molecular formula is C7H4F3NO2, molecular weight is 191.1074, as common compound, the synthetic route is as follows.Product Details of 80194-69-0

A mixture containing CoCl26H2O (12.40 mg, 0.05 mmol), Htpc (9.50 mg, 0.05 mmol),and water (6 mL) was sealed in a 15-mL Teflon-lined stainless steel vessel and heatedat 413 K for 3 days and then cooled to room temperature at a rate of 10 Kh1. Afterfiltration, red block crystals were collected and washed with distilled water severaltimes, then dried at room temperature. Yield: 4.96mg (40%, based on CoCl26H2O).Anal. Calcd (%) for C14H10CoF6N2O6 (molecular weight 475.17 gmol1): C, 35.39; H, 2.12; N, 5.90. Found (%): C, 35.54; H, 2.21; N, 5.98. IR (KBr, cm1): 3347 w, 1663 m,1510 m, 1410 m, 1148w, 936 w, 820 w, 640 w, 473 w.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,80194-69-0, 5-(Trifluoromethyl)picolinic acid, and friends who are interested can also refer to it.

Reference:
Article; Li, Bing; Wang, Jiakai; Song, Huan; Wu, Huanping; Chen, Xiaoyan; Ma, Xiaoxia; Journal of Coordination Chemistry; vol. 72; 15; (2019); p. 2562 – 2573;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 875232-70-5, 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.875232-70-5, name is 2,4-Dibromo-5-chloropyridine, molecular formula is C5H2Br2ClN, molecular weight is 271.3371, as common compound, the synthetic route is as follows.

Methyl 4′-amino-5′-methoxy-2′-methylbiphenyl-4-carboxylate generated in Step 1 (200 mg, 0.75 mmol), 2,4-dibromo-5-chloropyridine (222 mg, 0.82 mmol, 1.1 equiv), Pd2(dba)3 (17 mg, 0.02 mmol, 0.025 equiv.), xantphos (22 mg, 0.04 mmol, 0.05 equiv.), and Cs2CO3 (365 mg, 1.1 mmol, 1.5 equiv.) are added to THF (5 mL). The resulting mixture is bubbled with N2 gas for 5 minutes and then heated at 150 0C for 4 hours. After cooling to room temperature, the reaction mixture is diluted into EtOAc and washed with H2O. The EtOAc layer is dried over Mg2SO4 and concentrated in vacuo. Silica gel chromatography (hexanes-EtOAc) affords Methyl 4′-(4-bromo-5-chloropyridin-2-ylamino)-5′-methoxy-2′-methylbiphenyl-4-carboxylate; MS m/z 461.0 (M+l).

The chemical industry reduces the impact on the environment during synthesis 875232-70-5, I believe this compound will play a more active role in future production and life.

Reference:
Patent; IRM LLC; WO2008/73687; (2008); A2;,
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. 1173081-96-3, name is 3-(Aminomethyl)-4,6-dimethylpyridin-2(1H)-one hydrochloride. A new synthetic method of this compound is introduced below., category: pyridine-derivatives

0988] 3-{[(2R,4R,6S)-l-Benzyl-2,6-dimethylpiperidin-4-yl](ethyl)amino}-N-[(4,6- dimethyl-2-oxo-l,2-dihydropyridin-3-yl)methyl)-5-fluoro-2-methylbenzamide[0989] To a stirred solution of methyl 3-{ [(2R,4R,6S)-l -benzyl-2,6-dimethylpiperidin-4-yl] (ethyl)amino}-5-fluoro-2-methylbenzoate (48.5 mg, 0.1 18 mmol) in ethanol (1.5 mL) was added aq. NaOH (5 M, 47.0 ul, 0.235 mmol). The reaction mixture was stirred at 80 C for 1 .5 hours. After cooling to rt, solvent was removed in vacuo and dried under reduced pressure. To a stirred solution of this residue and 3-(aminomethyl)-4,6-dimethyl – l ,2-dihydropyridin-2-one HC1 salt (28.8 mg, 0.153 mmol) in DMSO ( 1 mL) was added PyBOP (91 .8 mg, 0.176 mmol) and Hunig’s base (102 ul, 0.588 mmol). The reaction mixture was stirred at 23C for 13.5 hours. The reaction mixture was quenched with water, and the mixture was extracted with ethylacetate. The organic layer was washed with water (2 10 mL) and brine (1 x 10 mL). The organic layer was dried over MgS04, filtered and the filtrate was concentrated in vacuo. The residue was purified by silica gel column chromatography (NH Si02, ethylacetate/MeOH=50/l to 8/1 ) to give title compound as a white solid (50.1 mg, 79% yield). MS(ES) [M+H] 533.3.

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, 1173081-96-3, 3-(Aminomethyl)-4,6-dimethylpyridin-2(1H)-one hydrochloride.

Reference:
Patent; EPIZYME, INC.; EISAI CO., LTD.; KUNTZ, Kevin, Wayne; CHESWORTH, Richard; DUNCAN, Kenneth, William; KEILHACK, Heike; WARHOLIC, Natalie; KLAUS, Christine; ZHENG, Wanjun; WO2012/142513; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 113975-31-8 ,Some common heterocyclic compound, 113975-31-8, molecular formula is C10H13IN2O, 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.

Manufacturing Example 1-2-3: 3-lodo-pyridin-2-ylamine N-(3-lodo-pyridin-2-yl)-2,2-dimethyl-propionamide (66.2 g, 218 mmol) described in Manufacturing Example 1-2-2, a 5 N aqueous solution (200 mL) of sodium hydroxide, and methanol (200 mL) were stirred under reflux for 1 hour and 20 minutes. The reaction solution was returned to room temperature, and then water was added thereto, which was extracted with ethyl acetate three times. The ethyl acetate layers were combined, which was washed once with saturated brine, and then dried over sodium sulfate. The sodium sulfate was removed by filtration, and the solvent was evaporated under a reduced pressure to obtain the titled compound (41 g). 1H-NMR spectrum (DMSO-d6) delta (ppm): 6.00 (2H, brs), 6.32 (1 H, dd, J = 4.8 Hz, 7.2 Hz), 7.87 (1 H, d, J = 7.2 Hz), 7.92 (1 H, d, J = 4.8 Hz).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,113975-31-8, its application will become more common.

Reference:
Patent; Eisai R&D Management Co., Ltd.; EP2065377; (2009); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 13602-11-4 ,Some common heterocyclic compound, 13602-11-4, molecular formula is C8H9NO2, 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.

INTERMEDIATE 88- PREPARATION of methyl 6-(bromomethyl)picolinate. A mixture of methyl 6-methylpicolinate (1.81 g; 1 1.97 mmol) and carbon tetrachloride (60 ml_) was treated with /V-bromosuccinimide (2.37 g, 13.17 mmol) and benzoyl peroxide (0.299 g; 1.20 mmol) and heated at refluxing temperature for 21 hours. The resulting brown suspension was concentrated under reduced pressure and the residue purified by flash chromatography on silica gel (eluent 0 to 6% ethyl acetate in dichloromethane) to give 0.773 g (28%) of methyl 6-(bromomethyl)picolinate as a white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,13602-11-4, its application will become more common.

Reference:
Patent; KATHOLIEKE UNIVERSITEIT LEUVEN, K.U. LEUVEN R&D; REMYND; GRIFFIOEN, Gerard; VAN DOOREN, Tom; ROJAS DE LA PARRA, Veronica; ALLASIA, Sara; MARCHAND, Arnaud; KILONDA, Amuri; CHALTIN, Patrick; WO2012/80221; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 1122-54-9, 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 1122-54-9, name is 4-Acetylpyridine. This compound has unique chemical properties. The synthetic route is as follows.

To a 9 sodium hydride (60% in 10 paraffin oil) (1.98g, 0.049mol), 10mL of 11 Dimethyl formamide was added dropwise at 5C under nitrogen atmosphere. To this mixture, 12 4-acetylpyridine (3.0g, 0.024mmol) was added dropwise and stirred for 30min at ambient temperature. Then 13 diethyl oxalate (4.03mL, 0.029mol) was added slowly and the reaction mixture was again stirred for 3h at room temperature. The completion of the reaction was monitored by TLC and quenched with crushed ice. Then the reaction mixture was extracted with ethyl acetate (1x100mL), washed with water (100mL) and brine solution (100mL). The organic layer was separated, dried over anhydrous sodium sulfate and evaporation of solvent affords the expected intermediate 14 1. (White solid, Yield 78%). 1H NMR (300MHz, CDCl3) delta 8.78 (d, J=5.5Hz, 2H), 7.85 (d, J=5.5Hz, 2H), 4.42 (q, J=14.0, 7.1Hz, 2H), 1.42 (t, J=7.0Hz, 3H). 13C NMR (75MHz, CDCl3) delta 192.89, 173.26, 165.10, 150.57, 137.70, 122.79, 61.75, 29.62, 14.15.

According to the analysis of related databases, 1122-54-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Madhu; Sivakumar; Journal of Photochemistry and Photobiology A: Chemistry; vol. 371; (2019); p. 341 – 348;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 114-33-0, 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. 114-33-0, name is N-Methylnicotinamide. A new synthetic method of this compound is introduced below.

General procedure: Complex 1 was prepared by the reaction of an aqueous solution of copper(II) acetate monohydrate (1mmol, 0.20g) with N-methylnicotinamide (2mmol, 0.27g) followed by addition of 4-fluorobenzoic acid (2mmol, 0.28g). The reaction mixture was stirred until a blue product was precipitated (3days). The fine blue microcrystals were filtered off, washed with a small portion of water and dried at ambient temperature. The mother liquor obtained from filtration were left to crystallize. The blue crystals suitable for X-ray structure determination were separated after several days. Yield: 0.41g (65%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,114-33-0, N-Methylnicotinamide, and friends who are interested can also refer to it.

Reference:
Article; Hala?ka, Jozef; Lokaj, Jan; Jomova, Klaudia; R??i?kova, Zde?ka; Mazur, Milan; Moncol, Jan; Polyhedron; vol. 175; (2020);,
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. 571189-16-7, name is tert-Butyl 4-(6-nitropyridin-3-yl)piperazine-1-carboxylate. This compound has unique chemical properties. The synthetic route is as follows. category: pyridine-derivatives

A nitrogen-flushed, 2.5 L heavy-wall Parr bottle (pressure rated to 60 psi) is charged with 68 g (0.22 mol,) of tert-butyl 4-(6-nitropyridin-3-yl)piperazine-1-carboxylate, (A2a), 6.8 g of 10% palladium on carbon, 50% water wet catalyst and 807 g (1020 mL) of methanol. The reaction vessel is inerted three times with nitrogen (ca. 30 psi), evacuating the atmosphere above the reaction mixture each time. The vessel is pressurized twice with hydrogen (ca. 30 psi), evacuating the atmosphere above the reaction mixture each time. The reaction vessel is pressurized to 45 psi with hydrogen. The shaker motor is started. The reaction is exothermic. A temperature rise from 19 to 54 C. over 15 min is observed after which time the hydrogen uptake stops. The mixture is allowed to cool to 30 C. over 1 h at which point the shaker is stopped. The hydrogen atmosphere is replaced with nitrogen as described above (Inert the reaction vessel). The catalyst is removed by filtration through a 10 g pad of filter cel. This entire process is repeated once more, both filtrates are combined and charged to a clean 3 L 4-neck round bottom flask.; The filtrates from Step 2.3 is stirred and concentrated under reduced pressure (50 mbar, 40 C. internal MAXIMUM.) to a thick paste. 190 g (250 mL) of tert-butyl methyl ether is charged to the residue. The sample is again stirred and concentrated under reduced pressure (50 mbar, 30 C. internal MAXIMUM.) to a thick paste. 342 g (500 mL) of heptane is charged to the residue and the resulting suspension is stirred for 15 min at 22+/-3 C. The solids are filtered and the filter cake is washed with 68 g (100 mL) of heptane. Dry the solids at 50 C. for 16 h, to afford 112.3 g (93.4%) of Compound A2 as tan plates, mp 124-126 C.

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, 571189-16-7, tert-Butyl 4-(6-nitropyridin-3-yl)piperazine-1-carboxylate.

Reference:
Patent; Calienni, John Vincent; Chen, Guang-Pei; Gong, Baoqing; Kapa, Prasad Koteswara; Saxena, Vishal; US2012/115878; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 848498-98-6 ,Some common heterocyclic compound, 848498-98-6, molecular formula is C8H8Cl2N2O2, 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.

[0365] l-(2,6-Dichloro-4-pyridinyl)ethanone (156). A solution of MeMgBr (3 M in Et2O, 4.3 mL, 12.8 mmol) was added slowly to a stirred solution of amide 155 (2.0 g, 8.5 mmol) in dry THF (40 mL) at 0 0C and the mixture was stirred at 0 0C for 3 h. The reaction mixture was quenched with aq. NH4Cl solution (15 mL) and the mixture extracted with EtOAc (3 x 50 mL). The combined organic fraction was washed with water (50 mL), washed with brine (50 mL), dried and the solvent evaporated. The crude product was recrystallized to give the ketone 156 as white crystals (1.61 g, 99%): mp (EtOAc) 50-51 C; 1H NMR (CDCl3) delta 7.68 (s, 2 H, H- 3′, H-5′), 2.61 (s, 3 H, H-2); MS m/z 190.4, 192.4 (MH+, 100, 70%).

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. 848498-98-6, 2,6-Dichloro-N-methoxy-N-methylisonicotinamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE BOARD OF TRUSTEES OF THE LELAND STANFORD JUNIOR UNIVERSITY; AUCKLAND UNISERVICES LIMITED; WO2009/114552; (2009); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 909036-46-0, 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. 909036-46-0, name is 2-Chloro-3-iodopyridin-4-amine. A new synthetic method of this compound is introduced below.

10.4 Synthesis of N-(2-chloro-3-iodo-pyridin-4-yl)methanesulfonamide 3a* 2-Chloro-3-iodo-pyridin-4-ylamine 2a* (5.1 g, 20 mmol) and triethylamine (14 mL, 100 mmol) were stirred in DCM (100 mL) and cooled in an ice water bath. Methanesulphonyl chloride (7.7 mL, 100 mmol) was added dropwise and stirred at room temperature for two h. The reaction mixture was washed with water (100 mL), dried over MgSO4 and concentrated in vacuo. The crude product was purified by column chromatography using 1% AcOEt in DCM to yield N-methanesulfonamide-N-(2-chloro-3-iodo-pyridin-4-yl)-methanesulfonamide (4.2 g, 51 %). 1H NMR (400 MHz, DMSO) delta(ppm): 8.53 (1 H, d, J = 5.1 Hz), 7.74 (1 H, d, J = 5.1 Hz), 3.70 (6 H, s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,909036-46-0, 2-Chloro-3-iodopyridin-4-amine, and friends who are interested can also refer to it.

Reference:
Patent; Max-Planck-Gesellschaft zur Foerderung der Wissenschaften e.V.; Ullrich, Axel (Prof. Dr.); Falcenberg, Mathias (Dr.); EP2818472; (2014); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem