Day: December 8, 2020

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 108-99-6 as follows., 108-99-6

Subsequently, 30g of the prepared catalyst were fed into a tube reactor having a diameter of 1 inch and a length of 5 centimeter to obtain a catalyst bed. 3-Methylpyridine was first mixed with air and then with H2O vapor and then continuously fed into the catalyst bed at a mole ratio of 1:45:145 (3-methylpyridine: oxygen: H2O) and where the bed temperature was controlled at 290C. The feed speed of 3-methylpyridine is 0.025 hr-1. The product was collected from output of the catalyst bed and analyzed by HPLC and GC. It was found that a conversion of 3-methylpyridine is 96.82%, a selectivity of nicotinic acid is 93.16%, and a selectivity of carbon dioxide is 6.76%. After continuous processing for 42 days, the catalyst was drawn out and examined by electronic microscopy. Its microscopic photograph was shown in Figure 7. From the Figure, it is known that according to the present process for preparing nicotinic acid by using the present catalyst, the crystal size of the active ingredients on the surface of carrier did not vary while time passed. Thus it demonstrates that the catalyst of the present invention exhibits excellent stability and longer lifetime. Moreover, as the crystal size of the active ingredients on the surface of the carrier is controlled in the range of from 40 to 100 nm by adding transition metal oxide, its catalytic activity increases. Thus a desired conversion and selectivity will be achieved by using less amount of catalyst.Example 8 The preparation of the catalyst of the present invention and the process for preparing nicotinic acid by using the catalyst 6.43 g of ammonium meta-vanadate were added into 500 ml water and the solution was heated at 70C to dissolve ammonium meta-vanadate. Then, 5.46 g of ammonium chromate were added into the solution and stirred for 30 minutes. Into the resultant solution were added 91.41 g titanium oxide (Degussa P-25) and stirred for 1 hour. The mixture was heated to evaporate water and then calcined in an oven at a temperature of 700C to obtain the catalyst of the present invention, whose composition was shown in Table 1. Subsequently, 30g of the prepared catalyst were fed into a tube reactor having a diameter of 1 inch and a length of 5 centimeter to obtain a catalyst bed. 3-Methylpyridine was first mixed with air and then with H2O vapor and then continuously fed into the catalyst bed at a mole ratio of 1:40:175 (3-methylpyridine: oxygen: H2O) and where the bed temperature was controlled at 305C. The feed speed of 3-methylpyridine is 0.02 hr-1. The product was collected at the outlet of the catalyst bed and analyzed by HPLC and GC. It was found that a conversion of 3-methylpyridine is 91.06%, a selectivity of nicotinic acid is 90.91 %, and a selectivity of carbon dioxide is 8.71%.Example 9 The preparation of the catalyst of the present invention and the process for preparing nicotinic acid by using the catalyst 3.21 g of ammonium meta-vanadate were added into 500 ml water and the solution was heated at 70C to dissolve ammonium meta-vanadate. Then, 2.73 g of ammonium chromate were added into the solution and stirred for 30 minutes. Into the resultant solution were added 95.71 g titanium oxide (Hembitec K-03) and stirred for 1 hour. The mixture was heated to evaporate water and then calcined in an oven at a temperature of 700C to obtain the catalyst of the present invention, whose composition was shown in Table 1. Subsequently, 30g of the prepared catalyst were fed into a tube reactor having a diameter of 1 inch and a length of 5 centimeter to obtain a catalyst bed. 3-Methylpyridine was first mixed with air and then with H2O vapor and then continuously fed into the catalyst bed at a mole ratio of 1:35:160 (3-methylpyridine: oxygen: H2O) and where the bed temperature was controlled at 265 C. The feed speed of 3-methylpyridine is 0.021 hr-1. The product was collected at the outlet of the catalyst bed and analyzed by HPLC and GC. It was found that a conversion of 3-methylpyridine is 92.99%, a selectivity of nicotinic acid is 88.75%, and a selectivity of carbon dioxide is 10.54%.

The chemical industry reduces the impact on the environment during synthesis 108-99-6, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Chang Chun Petrochemical Co. Ltd.; EP1584618; (2005); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

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 1603-41-4 as follows., 1603-41-4

Water (20 mL),3-Chloro-4- (4-methylphenyl) -4-oxobutanoic acid(5.02 g, 0.022 mol),2-Amino-5-methylpyridine (3) (3.58 g, 0.033 mol)And sodium carbonate (2.33 g, 0.022 mol) were successively added to a 100 mL reaction flask,After mixing,Slowly warmed to 80 internal temperature, nitrogen protection,Insulation reaction 7h, stop the reaction.With 6N hydrochloric acid pH = 0.5 ~ 1, Stirred at room temperature for 30min,No change in pH after the test, adding an equal amount of ethyl acetate,Stir 15min, points to the reservoir,Water layer plus activated carbon 0.1g, 50 decolorization 30min, hot filtration,The filtrate was adjusted to pH = 3.0 ~ 3.5 with 6N aqueous sodium hydroxide solution to precipitate a solid,Cooling to 0 ~ 5 insulation 1h, suction filtration, the filter cake with 10mL ice water rinse,80 vacuum drying 6h,3.21 g of pale yellow solid (HPLC: 97.6%) was obtained in a yield of 52.0%.

The chemical industry reduces the impact on the environment during synthesis 1603-41-4, I believe this compound will play a more active role in future production and life.

Reference:
Patent; East China University of Science and Technology; Zhao Jianhong; Guan Yu; Liao Fan; Deng Weiping; Shi Xiaoxin; Zhao Jinyuan; Ma Lirong; Chen Chunyan; Yang Jun; Li Jie; Lei Qingyun; (11 pag.)CN107383005; (2017); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

504-29-0, 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. 504-29-0, name is Pyridin-2-amine. A new synthetic method of this compound is introduced below.

a Pyridine-2-amino-5-sulphonic Acid 2-Aminopyridine (80 g, 0.85 mol) was added portionwise over 30 minutes to oleum (320 g) and the resulting solution heated at 140 C. for 4 hours. On cooling, the reaction was poured onto ice (200 g) and the mixture stirred in an ice/salt bath for a further 2 hours. The resulting suspension was filtered, the solid washed with ice water (200 ml) and cold IMS (200 ml) and dried under suction to afford the title compound as a solid, 111.3 g; LRMS: m/z 175 (M+1)+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,504-29-0, Pyridin-2-amine, and friends who are interested can also refer to it.

Reference:
Patent; Grossman, Eric B.; Koppiker, Nandan P.; Leichter, Steven B.; US2003/162782; (2003); 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. 1124-64-7, name is 1-Butylpyridinium Chloride, the common compound, a new synthetic route is introduced below. 1124-64-7

General procedure: A mixture of pyridine (0.80g, 10mmol) and bromoethane (1.30g, 12mmol) was stirred ar rt for 43h, then the mixture was washed with ether twice and treated with active charcoal for 12h by stirring. After removing active charcoal by filtration and washed with ether, the filtrate was dried under reduced pressure at rt to give 1-ethylpyridin-1-ium bromide (0.60g, 3.2mmol) in 32% yield. Mp 120C, 1H NMR (500MHz, ppm, CDCl3 J=Hz) delta 1.75 (3H, t, J=7.5), 5.10 (2H, q, J=7.5), 8.15 (2H, t, J=7), 8.53 (1H, s), 9.63 (2H, d, J=6.5); 13C NMR (125MHz, ppm, CDCl3 J=Hz) delta 17.37, 57.12, 57.39, 128.48, 128.64, 144.74, 144.92, 145.08, 145.60. A mixture of 1-ethylpyridin-1-ium bromide (150mg, 0.80mmol) and ammonium cetyl-PEG10 sulfate [20] (624mg, 0.80mmol) in dichloromethane (CH2Cl2) (8.0ml) was stirred at rt for 24h to form the precipitate of ammonium bromide (NH4Br). The precipitate was removed by filtration and the extract was diluted with CH2Cl2 and cooled to-25C to form the precipitate of NH4Br which was removed by filtration. This process was repeated several times until no more precipitate was formed. The resulting filtrate was dried by lyophilization to give 666mg (0.77mmol) of PYET in 96% yield

The synthetic route of 1124-64-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kadotani, Shiho; Nokami, Toshiki; Itoh, Toshiyuki; Tetrahedron; vol. 75; 4; (2019); p. 441 – 447;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

624-28-2, 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 624-28-2 as follows.

A 12L three-necked round-bottomed flask equipped with a mechanical stirrer and a condenser, connected on top with a nitrogen [BUBBLER] and a thermometer, was charged with 2,5-dibromopyridine (442 g, 1. [87MOLES),] hydrazine hydrate (55% wt., 1057 ml, [18.] 7 moles), poly (ethylene glycol) (average Mn about 300,1. 87 L), 2-butanol (373 [ML)] and water (1.87 L). The mixture was heated at reflux for 29 hours. The heating source was removed and the mixture was stirred for an additional 20 hours. To the resulting slurry, cold water [(2.] 2L) was added. The slurry was stirred for an additional [30] minutes and filtered. The cake was washed with cold water (3 x [200] [ML)] and dried in a vacuum-oven [(40C)] for 48 hours. The title compound was obtained as off-white flakes (305 g, yield 87%). GCMS (m/z): 187 (M+). [H’NMR] (400 MHz, [CDCI3)] : 8 8.14 (d, J=2.0 Hz, 1H), 7.55 (dd, J=8.7/2. 0 Hz, 1 H), 6.66 (d, J=8.7Hz, [1 H),] 5.89 (brs, 1 H), 3.65 (brs, 2H).

The chemical industry reduces the impact on the environment during synthesis 624-28-2, I believe this compound will play a more active role in future production and life.

Reference:
Patent; PFIZER PRODUCTS INC.; WO2004/20438; (2004); A2;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

141-86-6, 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. 141-86-6, name is 2,6-Diaminopyridine, molecular formula is C5H7N3, 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: Diamine (1mmol), alcohol (2mmol), catalyst (1mol %), KOH (50mol %) and toluene (2mL) were placed in a 25mL round bottomed flask and stirred on a preheated oil bath (100C) for 12h. Upon completion (as monitored by TLC), the reaction mixture was cooled at ambient temperature, H2O (3mL) was added and the organic layer was extracted with ethyl acetate. The organic extract was separated, dried, and concentrated. The desired product was purified by column chromatography with CH2Cl2/EtOAc as eluent.

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. 141-86-6, 2,6-Diaminopyridine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ramachandran, Rangasamy; Prakash, Govindan; Nirmala, Muthukumaran; Viswanathamurthi, Periasamy; Malecki, Jan Grzegorz; Journal of Organometallic Chemistry; vol. 791; (2015); p. 130 – 140;,
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. 108-99-6, name is 3-Methylpyridine. This compound has unique chemical properties. The synthetic route is as follows. 108-99-6

Example 5 The preparation of the catalyst of the present invention and the process for preparing nicotinic acid by using the catalyst 6.43 g of ammonium meta-vanadate were added into 500 ml water and the solution was heated at 70C to dissolve ammonium meta-vanadate. Then, 13.54 g of ferric nitrate were added into the solution and stirred for 30 minutes. Into the resultant solution were added 92.31 g titanium oxide (Hembitec K-03) and stirred for 1 hour. The mixture was heated to evaporate water and then calcined in an oven at a temperature of 700C to obtain the catalyst of the present invention, whose composition was shown in Table 1. After calcination, the catalyst was observed by electronic microscopy and found that the crystal size of the active ingredients on the surface of the carrier is from 60 to 80 nm, as shown in Figure 11. Subsequently, 30g of the prepared catalyst were fed into a tube reactor having a diameter of 1 inch and a length of 5 centimeter to obtain a catalyst bed. 3-Methylpyridine was first mixed with air and then with H2O vapor and then continuously fed into the catalyst bed at a mole ratio of 1:35:330 (3-methylpyridine: oxygen: H2O) and where the bed temperature was controlled at 310C. The feed speed of 3-methylpyridine is 0.02 hr-1. The product was collected at the outlet of the catalyst bed and analyzed by HPLC and GC. It was found that a conversion of 3-methylpyridine is 96.78%, a selectivity of nicotinic acid is 93.13%, and a selectivity of carbon dioxide is 5.56%.

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, 108-99-6, 3-Methylpyridine.

Reference:
Patent; Chang Chun Petrochemical Co. Ltd.; EP1584618; (2005); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

13472-85-0, 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 13472-85-0, name is 5-Bromo-2-methoxypyridine. This compound has unique chemical properties. The synthetic route is as follows.

Example 4: Synthesis of 3-(5-hydroxy-3-(2-methyl-2-propylthio)-l-[4[(2-methoxypyridin-5-yl)benzyl]- indol-2-yl-2,2-dimethyl-propionic acid ethyl ester (R = -CH2CH3; X = Br). Ethyl 3-(3-(tert-butylthio)-5-hydroxy-l-(4-(4,4J5,5-tetramethyl-l,3,2-dioxaborolan-2-yl)benzyl)-lH- indol-2-yl)-2,2-dimethylpropionate (675g, 1.2 mol), 5-bromo-2-methoxypyridine (280.5g, 1.5 mol), Pd(PPh3)4(23.63g, 0.02 mol), and K2CO3 (412g) were added to a reactor containing 6.75 L of DME and 3.38 L of water and stirred. Nitrogen gas was bubbled into the mixture for about 20 minutes. The mixture was then heated to between 80 to 85 0C and stirred overnight. TLC analysis (EtO Ac/Petroleum ether = 1/5) showed the reaction had reached completion. The mixture was subsequently cooled to ambient temperature. Following cooling, the compound was extracted three times with EtOAc. The organic layer was then washed with water, followed by a brine wash. The organic layer was then dried with sodium sulfate, the solid removed by filtration and the organic layer was then concentrated in vacuo, affording 653 g of product in near quantitative yield.

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 13472-85-0, 5-Bromo-2-methoxypyridine.

Reference:
Patent; AMIRA PHARMACEUTICALS, INC.; WO2009/55721; (2009); A2;,
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 641569-94-0, name is 4-Methyl-3-((4-(pyridin-3-yl)pyrimidin-2-yl)amino)benzoic acid. This compound has unique chemical properties. The synthetic route is as follows. 641569-94-0

Add 4-Methyl-3-[[4- (3-pyridinyl) -2-pyrimidinyl] amino] benzoic acid (107.2 mg, 0.35 mmol), add thionyl chloride (0.50 mL), DMF (3 drops) and bring to room temperature The mixture was stirred for 17 hours. The solution was then concentrated to dryness.After that, THF (5.0 mL) was added and 3-Bromo-4- (4-methyl-piperazin-1-ylmethyl) -phenylamine (C) (82.4 mg, 0.29 mmol),DMAP (1.2 mg, 0.01 mmol),N, N-Diisopropylethylamine (60.6 muL, 0.35 mmol) was added and the mixture was stirred at room temperature for 2.5 hours. Add water and ethyl acetate,After washing with saturated aqueous sodium hydrogen carbonate solution, the solvent was distilled off. The obtained residue is subjected to silica gel column chromatographyPurification by (chloroform: methanol = 5: 1) gave IMT-5 precursor (43.0 mg, 0.075 mmol, 25%, white solid)

Statistics shows that 641569-94-0 is playing an increasingly important role. we look forward to future research findings about 4-Methyl-3-((4-(pyridin-3-yl)pyrimidin-2-yl)amino)benzoic acid.

Reference:
Patent; Kyoto University; Arkray Corporation; Saji, Hideo; Kimura, Hiroyuki; Matsuda, Hirokazu; Soma, Tasukukei; Nakanishi, Shuichi; (26 pag.)JP2019/64987; (2019); A;,
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. 141-86-6, name is 2,6-Diaminopyridine. This compound has unique chemical properties. The synthetic route is as follows. 141-86-6

Preparation 44. N- (6-Amino-pyridin-2-yl) acetamide; Dissolve 2,6-diaminopyridine (9.822 g, 90 mmol) in dioxane (100 mL) and cool to 0C. Add acetyl chloride (2.355 g, 2.1 mL, 30 mmol) slowly and stir for 1 hr. at 0C. Remove the ice bath and stir at room temperature overnight. Quench the reaction mixture with saturated NaHCO3 solution, extract with ethylacetate three times. Combine the organic layers, dry over Na2S04, filter, and concentrate to give a solid. Chromatography on silica gel, eluting with a gradient of 60-70% ethylacetate in hexanes affords the title intermediate (3.45 g, 76%): mass spectrum (ion spray): m/z = 152. 1 (M+1) ; 1H NMR (CDC13, ppm): 7.49 (m, 3H), 6.28 (d, 1H), 4.31 (s, br, 2H), 2.19 (s, 3H).

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, 141-86-6, 2,6-Diaminopyridine.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/35499; (2005); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem