Tag: M.W=0-100

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 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 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. 626-64-2, name is Pyridin-4-ol, the common compound, a new synthetic route is introduced below. 626-64-2

A solution of an alcohol (0.4 mmol), a phenol/thiophenol (0.4 mmol), diisopro-pylethylamin (0.44 mmol) and tributylphosphine (0.52 mmol) in THF (5 mL) was stirred undernitrogen at rt. 1,1′-(Azodicarbonyl)dipiperidine (ADDP, 0.52 mmol) dissolved in THF (5 mL)was added and the reaction mixture was stirred at rt for 16 h. The reaction mixture was fil- tered and the filtrate was evaporated to dryness, which gave a crude which was either puri- fied by flash chromatography (Quad flash 25, EtOAc-heptane) or redissolved in MeCN andpurified by preparative HPLC (Gilson).Example 1 (General procedure 1)Methyl-phenyl-carbamic acid 4-[2-(pyridin-4-yloxy)-ethyl]-phenyl esterThe title compound (99%) was prepared as an oil using methyl-phenyl-carbamic acid 4-(2-hydroxy-ethyl)-phenyl ester and 4-hydroxypyridine.HPLC-MS : mlz = 349.2 (M+1); R, = 2.64 min.

Statistics shows that 626-64-2 is playing an increasingly important role. we look forward to future research findings about Pyridin-4-ol.

Reference:
Patent; NOVO NORDISK A/S; WO2004/111006; (2004); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

462-08-8, 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. 462-08-8, name is Pyridin-3-amine, the common compound, a new synthetic route is introduced below.

Example 28 Manufacturing t-butyl pyridin-3-ylcarbamate Into a solution obtained by dissolving 100.0 g (1.06 mol) of 3-aminopyridine in a mixed solvent of 300 ml of 2-propanol and 100 mL of water, a mixed solution of 266.7 g (1.22 mol) of di-t-butyl dicarbonate and 100 mL of 2-propanol was added dropwise over three hours. The inner temperature of the mixture during the dropwise addition was maintained to be 5 to 20C. After the dropwise addition was finished, the obtained mixture was stirred at room temperature for 3 hours, and the resultant was subjected to a concentration process under reduced pressure. To the concentration residue, 200 mL of water was added. After the resultant was further subjected to a concentration process, 200 mL of water was added to the concentration residue, and the deposited crystals were filtered. The obtained crystals were washed with 200 ml of water to obtain 234.2 g of hydrous crystals of t-butyl pyridin-3-ylcarbamate. The hydrous crystals were analyzed by gas chromatography with a result that the content of t-butyl pyridin-3-ylcarbamate was 79.5 wt%, with a yield of 90.2%.

Statistics shows that 462-08-8 is playing an increasingly important role. we look forward to future research findings about Pyridin-3-amine.

Reference:
Patent; Sumitomo Chemical Company, Limited; EP2269986; (2011); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

504-29-0, 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. 504-29-0, name is Pyridin-2-amine. This compound has unique chemical properties. The synthetic route is as follows.

S1. Dichloromethane (900 g) was added to a 2 L three-neck bottle at room temperature. 2-Aminopyridine (135 g, 1.0 eq), triethylamine (174 g, 1.2 eq), Cool down to 10-20 C, add pivaloyl chloride (189 g, 1.1 eq), After the addition is completed, the system is warmed to 20-25 C, and the reaction is 2-3 h; After the reaction was completed, water was added to the reaction system, and after stirring for 0.5 h, the organic phase was separated. The aqueous phase was extracted with dichloromethane (500 g). Add petroleum ether (800g) directly at 0 C, stir for 2 h, suction filtration, 2-Pentylaminopyridine was obtained in a yield of 83%.

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, 504-29-0, Pyridin-2-amine.

Reference:
Patent; Aisite (Chengdu) Bio-pharmaceutical Co., Ltd.; Luo Jianye; Li Hongqiang; Guo Peng; (10 pag.)CN108675954; (2018); A;,
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 462-08-8 as follows., 462-08-8

To a flame-dried 500 mL round-bottom flask purged with N2 was added 3- aminopyridine (10.0 g, 105 mmol) and THF (109 mL). NaHMDS (210 mL, 1.0 M solution in THF, 210 mmol) was added dropwise over 1 h and the resulting red solution was stirred for 30 min. Di-tert-butyl dicarbonate (24.3 mL, 105 mmol) was added dropwise over 2 min. After 19 h, the dark red solution was concentrated to 100 mL and H2O (1.0 L) was added. The mixture was extracted with EtOAc (3×500 mL). The combined organic layers were washed with brine, dried (MgSO4) and concentrated to give product (19.9 g, 102 mmol, 97%) as a brown solid: 1H NMR (CDCl3, 400 MHz) 8.46 (d, J = 2.5 Hz, 1 H), 8.31 (dd, J = 4.7, 1.4 Hz, 1 H), 8.00 (d, J = 6.7 Hz, 1 H), 7.26 (dd, J = 8.4, 4.7 Hz, 1 H), 6.65-6.66 (m, 1 H) 1.55 (s, 9 H).

The chemical industry reduces the impact on the environment during synthesis 462-08-8, I believe this compound will play a more active role in future production and life.

Reference:
Patent; UNIVERSITY OF PITTSBURGH – OF THE COMMONWEALTH SYSTEM OF HIGHER EDUCATION; HURYN, Donna M.; WIPF, Peter; LAPORTE, Matthew G.; (137 pag.)WO2018/209083; (2018); 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 626-64-2 as follows., 626-64-2

Under nitrogen, 7-bromo-4-hydroxy-1-methyl-2-oxo -1,2-dihydro-quinoline-3-carboxylic acid methyl ester (1.00g, 3 . 2mmol), pyridin-4-ol (0.432g, 4 . 54mmol), N, N-dimethyl glycine (0.088g, 0 . 85mmol), cuprous iodide (0.082g, 0 . 43mmol), cesium carbonate (2.50g, 7 . 67mmol) and N, N-dimethylformamide (20 ml) were added in the flask. The reaction mixture is heated to 140 C for 12 hours. Cooling to room temperature, adding ice water (40 ml), using 1M pH=6 dilute hydrochloric acid is adjusted to, filtration, filters the filtrate, dry to give a white solid (1.05g, 100%).

The chemical industry reduces the impact on the environment during synthesis 626-64-2, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Guangdong East Sunshine Pharmaceutical Co., Ltd.; Zhuo, Yinglin; Wang, Xiaojun; Zhang, Yingjun; Wen, Liang; Wu, Shoutao; Yuan, Xiaofeng; (87 pag.)CN105384687; (2016); 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. 626-64-2, name is Pyridin-4-ol. A new synthetic method of this compound is introduced below., 626-64-2

Add 10.6 g (0.10 mol) of Na2CO3 and 12.7 g (0.05 mol) of I2 to a solution of 4.76 g (0.05 mol) pyridin-4-ol in 200 ml of water. Stir the reaction mass at room temperature for 12 h; use the TLC method to ensure the completeness of the reaction. Add 12 ml of HCl to =5, Na2S2O3 till color removal. Filtrate the resulting precipitate, mix the precipitate with 200 ml of boiling ethanol and filtrate one more time. Concentrate the filtrate under reduced pressure, re-crystallize residue from methanol. Yield: 3.4 g (31%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,626-64-2, Pyridin-4-ol, and friends who are interested can also refer to it.

Reference:
Patent; JOINT STOCK COMPANY “BIOCAD”; GAVRILOV, Aleksey Sergeevich; ALESHUNIN, Pavel Aleksandrovich; GORBUNOVA, Svetlana Leonidovna; REKHARSKY, Mikhail Vladimirovich; KOZHEMYAKINA, Natalia Vladimirovna; KUKUSHKINA, Anna Aleksandrovna; KUSHAKOVA, Anna Sergeevna; MIKHAYLOV, Leonid Evgen`evich; MOLDAVSKY, Alexander; POPKOVA, Aleksandra Vladimirovna; SILONOV, Sergey Aleksandrovich; SMIRNOVA, Svetlana Sergeevna; IAKOVLEV, Pavel Andreevich; (197 pag.)WO2018/92047; (2018); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

462-08-8, 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. 462-08-8, name is Pyridin-3-amine, molecular formula is C5H6N2, 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.

50.0 g (0.53 mol) of 3-aminopyridine was added to 34.9 g of 35percent hydrochloric acid and stirred to prepare an aqueous hydrochloric acid solution of 3-aminopyridine. In addition, 35.9 g (0.52 mol, 0.98 mol equivalent to 3-aminopyridine) of sodium nitrite was added to 54.0 g of water and stirred to prepare an aqueous solution of sodium nitrite. 131 g of hydrochloric acid was placed in a 500 mL four-necked brown colben and cooled to -20 ¡ã C. An aqueous hydrochloric acid solution of 3-aminopyridine and an aqueous solution of sodium nitrite were simultaneously added dropwise to hydrochloric acid in a temperature range of -20 ¡À 2 ¡ã C. over 2 hours with stirring. After completion of the dropwise addition, the mixture was further stirred for 30 minutes in a temperature range of -20 ¡À 2 ¡ã C. to obtain an aqueous solution of pyridine-3-diazonium salt650 g of dichloromethane was placed in 1000 mL four-necked brown bottle and cooled to 0 ¡ã C., and 119 g (1.86 mol) of sulfur dioxide gas was blown into the solution to dissolve. 0.9 g (0.006 mol) of copper (II) chloride dihydrate was added and cooled to -5 ¡ã C., and an aqueous solution of pyridine-3-diazonium salt was added over a period of 1 hour at a temperature range of -5 ¡À 2 ¡ã C. Was added dropwise. After completion of the dropwise addition, the mixture was further stirred for 1 minute at a temperature range of -5 ¡À 2 ¡ã C. The copper catalyst was removed by filtration while maintaining the temperature of the reaction solution at -5 ¡À 5 ¡ã C., and then the organic layer and the aqueous layer were separated. It was extracted with 195 g of dichloromethane ¡Á 3 times at a temperature of -5 ¡À 5 ¡ã C. and mixed all together to obtain 1353 g of an organic layer. GC analysis of this organic layer revealed that the concentration of pyridine-3-sulfonyl chloride was 3.76percent by mass and the yield was 54.0percent. The obtained organic layer was washed with 50 g of water while maintaining the temperature at 3 ¡À 2 ¡ã C., and then dehydrated using 20 g of magnesium sulfate at room temperature. After removing the magnesium sulfate by filtration, the filtrate was concentrated under reduced pressure (30 to 35 ¡ã C.,> 67 kPa) to remove dichloromethane. Subsequently, distillation under reduced pressure (110 ¡ã C., 1.3 kPa) gave 49.0 g (0.276 mol, yield 52.1percent) of pyridine-3-sulfonyl chloride.

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. 462-08-8, Pyridin-3-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Tama Chemical Industry Co., Ltd.; Nobushima, Hirofumi; Kobayashi, Hitoshi; (9 pag.)JP2016/175885; (2016); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

504-29-0, 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. 504-29-0, name is Pyridin-2-amine, the common compound, a new synthetic route is introduced below.

General procedure: To a solution of aniline (1 mmol) in THF (10 mL) were added triethylamine (2 mmol) and pivaloyl chloride (1.2 mmol) at 0 C under inert atmosphere. After stirring for 12 h at room temperature, the triethylammonium chloride was removed by filtration and the filtrate was evaporated under reduced pressure to afford crude product which was washed with heptane to afford pure N-pivaloyl anilines.

Statistics shows that 504-29-0 is playing an increasingly important role. we look forward to future research findings about Pyridin-2-amine.

Reference:
Article; Kathiravan, Subban; Nicholls, Ian A.; Tetrahedron Letters; vol. 58; 1; (2017); p. 1 – 4;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem