Tag: M.W:100-200

Reference of 96630-88-5, 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.96630-88-5, name is 4-Chloro-3-hydroxypyridine, molecular formula is C5H4ClNO, molecular weight is 129.5444, as common compound, the synthetic route is as follows.

a) A solution of diazenedicarboxylic acid diethyl ester (0.1572 mol) in THF (163 ml) was added dropwise to a mixture of 4-chloro-3-pyridinol (0.1429 mol), 2-propen-1-ol (0.1572 mol) and triphenyl-phosphine (0.1572 mol) in THF (276 ml), that was cooled with an ice-water bath and under nitrogen flow.The formed mixture was stirred on the ice-water bath for 15 minutes and at room temperature overnight.The mixture was concentrated under vacuum and the residue was washed with a saturated Na2CO3- solution.The mixture was extracted with DCM and the separated organic layer was dried, filtered and the solvent was evaporated until dry.The residue was treated with DIPE and the formed solid was filtered off and discarded.The filtrate was evaporated until dry and the residue was treated with diethyl ether and the formed solid was filtered off and discarded again.The filtrate was evaporated until dry and the residue was purified by open column chromatography over silica gel (eluent: DCM/2-propanone 99/1;98/2).The product fractions were collected and the solvent was evaporated, yielding 7.9 g of 4-chloro-3-(2-propenyloxy)-pyridine (intermediate (44).

The chemical industry reduces the impact on the environment during synthesis 96630-88-5, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Van Emelen, Kristof; De Bruyn, Marcel Frans Leopold; Alcazar-Vaca, Manuel Jesus; Andres-Gil, Jose Ignacio; Fernandez-Gadea, Francisco Javier; Matesanz-Ballesteros, Maria Encarnacion; Bartolome-Nebreda, Jose Manuel; US2004/19051; (2004); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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.2369-19-9, name is 2-Fluoro-5-methylpyridine, molecular formula is C6H6FN, molecular weight is 111.1169, as common compound, the synthetic route is as follows.category: pyridine-derivatives

Diisopropylamine (910.7 mg, 1.261 mL, 9.000 mmol) was dissolved in dry TetaF(20mL) and cooled to -78 0C, n-Buli (3.600 mL of 2.5 M, 9.000 mmol) was added slowly dropwise and the resultant mixture was then allowed to warm to -20 0C over 40min before being cooled back down to -78 0C.[ 00363 ] A solution of 2-fluoro-5-methyl-pyridine (1.0 g, 9.000 mmol) in dry THF(1OmL) was added dropwise and the solution was stirred at this temp for 2 hours. A solution of iodine (2.284 g, 463.3 muL, 9.000 mmol) in THF (1OmL) was then added and the resultant mixture stirred for a further 1 hour at this temp before being quenched with water. The resulting mixture was partitioned between sodium thiosulfate solution and Et2theta, organics separated and washed further with saturated NaCl. The combined organics were dried over Na2SO4, filtered and concentrated under reduced pressure to give a colourless oil. The resulting mixture was purified by column chromatography (30% EtOAc in hexanes, ~200mL silica) to give a colourless foam (1.409g, 66% Yield). 1 H NMR (400.0 MHz, DMSO) d 1 .42 (s, 1 H) and 7.07 – 7.12 (s, 2H) ppm

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2369-19-9, 2-Fluoro-5-methylpyridine, and friends who are interested can also refer to it.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; WO2009/73300; (2009); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 19346-43-1, Adding some certain compound to certain chemical reactions, such as: 19346-43-1, name is 2-Fluoro-3-nitro-4-picoline,molecular formula is C6H5FN2O2, 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 19346-43-1.

1. Preparation of 3-Amino-2-fluoro-4-methylpyridine To a solution of 10.1 g (grams) (65 mmol (millimole)) of 2-fluoro-4-methyl-3-nitropyridine in 200 mL (milliliter) of ethyl acetate was added 25 g (0.40 mol) of acetic acid and 0.8 g of 5 percent palladium on carbon catalyst. This mixture was shaken under 50 psig (pounds per square inch gauge, 2400 kiloPascals) pressure of hydrogen for 18 hours, was filtered, and was concentrated by evaporation under reduced pressure to obtain an oil. This oil was partitioned between dilute aqueous sodium bicarbonate and ether. The organic phase was separated, dried over magnesium sulfate, and filtered. The filtrate was concentrated by evaporation under reduced pressure and the residue was purified by column chromatography to obtain 7.2 g (88 percent of theory) of the title compound as a colorless solid melting at 63-64 C. Elemental Analysis C6 H7 FN2 Calc.: %C, 57.1; %H, 5.59; %N, 22.2 Found: %C, 57.2; %H, 5.73; %N, 22.1 1 H NMR (nuclear magnetic resonance spectrum (200 megahertz)) CDCl3:7.4 (d, 1H, J=5.0); 6.8 (d, 1H, J=5.0); 3.7 (br, 2H); 2.1 (s, 3H); 13C NMR CDCl3:152.6 (d, J=229); 134.1 (d, J=8.6); 133.8 (d, J=14.5); 128.1 (d, J=27.1); 123.3, 16.4 (d, J=4.1).

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. 19346-43-1, 2-Fluoro-3-nitro-4-picoline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DowElanco; US5614469; (1997); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 188577-68-6, 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. 188577-68-6, name is 4,5-Dichloropyridin-2-amine, molecular formula is C5H4Cl2N2, 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.

[0928] To a solution of phosgene (20% solution in toluene,0.186 ml, 0.353 mmol) in THF (2 ml) was added triethylamine(0.141 ml, 1.01 mmol). To the resulting white suspensionwas added a solution of 7-(dimethoxymethyl)-1,2,3,4-tetrahydro-1,8-naphthyridine (intermediate 4, 70 mg, 0.336mmol) in THF (2 ml) drop wise. The resulting yellow suspensionwas stirred at room temperature for 1 h. 4,5-dichloropyridin-2-amine (65.7 mg, 0.403 mmol) in THF (1 ml) wasadded to the mixture and stirred at room temperature for 16 h.The reaction mixture was filtered through a silica gel plug andwashed with heptanes/EtOAc 1:1 (35 ml), the filtrate wasconcentrated. The residue was dissolved in dioxane (1 ml)and treated with HCl (4 Min dioxane, 1 ml, 4.0 mmol). Themixture was stirred at room temperature for 2 h, diluted withDCM and quenched with saturated aqueous NaHC03 . Theorg. layer was collected and the water layer was extractedwith DCM. The combined org. layers were dried over anhydrousNa2S04 and concentrated under reduced pressure. Thecrude product was dissolved in acetonitrile/NMP/TFA, filteredthrough a syringe filter (0.2 f.tm) and purified by preparativereverse phase LC-MS (RP 1). The clean fractionswere combined and lyophilized to obtain the title compoundas an off 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 188577-68-6, 4,5-Dichloropyridin-2-amine.

Reference:
Patent; Novartis AG; Buschmann, Nicole; Fairhurst, Robin Alec; Furet, Pascal; Knoepfel, Thomas; Leblanc, Catherine; Liao, Lv; Mah, Robert; Nimsgern, Pierre; Ripoche, Sebastien; Xiong, Jing; Han, Bo; Wang, Can; Zhao, Xianglin; US2015/119385; (2015); 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 72141-44-7, name is 4-Chloro-2-methoxypyridine. This compound has unique chemical properties. The synthetic route is as follows. category: pyridine-derivatives

To a solution of compound 2 (28.7 g. 0.2 mol) in DMF (50 mL) was added NBS (35.5 g, 0.2 mol). The mixture was heated at 90C for 8 hours. The crude compound 3 was collected by filtration. (22 g, 50% yield).

With the rapid development of chemical substances, we look forward to future research findings about 72141-44-7.

Reference:
Patent; INTERMUNE, INC.; RAMPHAL, Johnnie, Y.; BUCKMAN, Brad, Owen; EMAYAN, Kumaraswamy; NICHOLAS, John, Beamond; SEIWERT, Scott, D.; WO2015/153683; (2015); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Synthetic Route of 4214-74-8 ,Some common heterocyclic compound, 4214-74-8, molecular formula is C5H4Cl2N2, 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.

PREPARATION 4 Preparation of 2-bromo-3,5-dichloropyridine 2-Bromo-3,5-dichloropyridine was prepared from 2-amino-3,5-dichloropyridine according to the method of L. C. Craig, J. Amer. Chem. Soc., 1934, 56, 231 to furnish a pale yellow crystalline solid in 76% yield, m.p. 37-38 C.

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. 4214-74-8, 3,5-Dichloropyridin-2-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Pfizer Inc.; US4510148; (1985); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 6623-21-8, 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 6623-21-8, name is 4,6-Dimethylnicotinonitrile. This compound has unique chemical properties. The synthetic route is as follows.

4,6-Dimethylnicotinonitrile (1.0 g, 7.6 mmol) was dissolved in ethanol (35 mL) and the mixture was treated with Raney nickel (5 mL, slurry in water) and hydrazine hydrate (3.8 mL, 75.6 mmol). The solution was stirred overnight at room temperature. Compound 2a was obtained by filtering the reaction mixture through a pad of diatomaceous earth, which was rinsed with methanol (3×50 mL). The filtrate was dried over Na2SO4, filtered and concentrated under reduced pressure to afford Compound 2a. The compound was used without additional purification. M+(ES+)=137.1 1H NMR (DMSO, d6) delta 2.35 (s, 3H), 2.42 (s, 3H), 4.01 (s, 2H), 7.13 (s, 1H), 8.42 (s, 1H).

According to the analysis of related databases, 6623-21-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Flores, Christopher M.; Wade, Paul R.; US2011/319400; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 22620-32-2, 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. 22620-32-2, name is (5-Fluoropyridin-3-yl)methanol. A new synthetic method of this compound is introduced below.

To a solution of (5-fluoropyridin-3-yl)methanol (430 mg, 3.4 mmol) in anhydrous dichloromethane (30 mL) was added dropwise phosphorus tribromide (650 muL, 6.8 mmol). The mixture was stirred at room temperature overnight. Dichloromethane was evaporated. The residue was dried in vacuo, affording 3-(bromomethyl)-5- fluoropyridine hydrobromide. The product was used without further purification.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,22620-32-2, (5-Fluoropyridin-3-yl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; CHLORION PHARMA, INC.; UNIVERSITE LAVAL; ATTARDO, Giorgio; TRIPATHY, Sasmita; WO2010/132999; (2010); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 62002-31-7, 4,5,6,7-Tetrahydro-3H-imidazo[4,5-c]pyridine dihydrochloride, 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, Safety of 4,5,6,7-Tetrahydro-3H-imidazo[4,5-c]pyridine dihydrochloride, blongs to pyridine-derivatives compound. Safety of 4,5,6,7-Tetrahydro-3H-imidazo[4,5-c]pyridine dihydrochloride

At 0 C., EDC (0.45 g, 2.4 mmol) was added to a solution of 1-hydroxy-7-azabenzotriazole (0.32 g, 2.4 mmol) and 2-norbornaneacetic acid (0.338 mL, 2.4 mmol) in dichloromethane (30 mL). The reaction mixture was stirred for 20 min at 0 C. 4,5,6,7-Tetrahydroimidazo[4,5-c]pyridine dihycrochloride (0.50 g, 2.3 mmol) was added. Ethyldiisopropylamine (0.40 mL, 2.3 mmol) was added. The reaction mixture was stirred for 16 h at room temperature. It was diluted with ethyl acetate (100 mL) and washed with a saturated aqueous solution of sodium hydrogencarbonate (100 mL). The aqueous solution was extracted with ethyl acetate (2*60 mL). The combined organic layers were dried over magnesium sulfate. The solvent was removed in vacuo. The crude product was purified by flash chromatography on silica (40 g), using dichloromethane/methanol/25% aqueous ammonia (100:10:1) as eluent, to give 120 mg of the title compound. 1H NMR (CDCl3, 2 rotamers): delta 1.00-2.50 (m, 13H); 2.65 and 2.75 (both t, together 2H); 3.75 and 3.90 (both t, together 2H); 4.55 and 4.65 (both s, together 2H); 7.53 (s, 1H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,62002-31-7, 4,5,6,7-Tetrahydro-3H-imidazo[4,5-c]pyridine dihydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; Novo Nordisk A/S; US6908926; (2005); B1;,
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. 56673-34-8, name is 3-Bromo-6-mercaptopyridine, molecular formula is C5H4BrNS, 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. Formula: C5H4BrNS

A suspension of 5-bromo-pyridine-2-thiol (which may be prepared as described for Intermediate 1.05; 2 g, 10.5 mmol) in carbon tetrachloride (40 mL) and water (8 mL) was cooled to 0 C. using an ice-bath. Chlorine gas was bubbled through the reaction mixture for 20 min and then CH2Cl2 (100 mL) was added. The mixture was washed with brine. The organic layer was dried over anhydrous Na2SO4, filtered, and evaporated under reduced pressure to give 5-bromo-pyridine-2-sulfonyl chloride (1.92 g, 71%) as a light yellow solid which was used directly in the next step without further purification. NMR (400 MHz, DMSO-d6) delta: 8.63 (d, J=1.5 Hz, 3H), 8.07 (dd, J=8.3, 2.2 Hz, 3H), 7.68 (d, J=8.3 Hz, 3H).

With the rapid development of chemical substances, we look forward to future research findings about 56673-34-8.

Reference:
Patent; Firooznia, Fariborz; Gillespie, Paul; Lin, Tai-An; So, Sung-Sau; US2012/309796; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem