Category: 108-99-6

Application of 108-99-6 ,Some common heterocyclic compound, 108-99-6, molecular formula is C6H7N, 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.

Example 2; The pelletized catalyst, TOSOH HSZ-690 HOD (SAR 203) with a silica binder, was ground to a coarse powder and screened to obtain a uniform size of 1-2 mm in diameter. A weight of 0.26 g of catalyst was charged into the reactor tube and glass wool (Pyrex) was used to secure it in place. Operating at a chlorine feed of 5 cc/min, a beta-picoline feed rate of 0.13 mg/min (10 cc/min N2 with a chiller temperature of 10 C.), the reagents were fed to the reactor at an initial temperature of 250 C. The system was initially ramped up to 325 C. and allowed to stablize. Under these conditions the product gases were 18.5% 3-trichloromethylpyridine (beta-tri ) and 65.4% beta-2-tet. When the system was allowed to stabilized at 350 C. the amount of beta-tri in the product gases was reduced to 2.6% and the conversion to beta-2-tet increased to 68.6% (see Table 2).; Example 3; The catalyst, TOSOH HSZ-690 HOD (SAR 203) with the silica binder, was sized to a uniform particle size of 1-2 mm in diameter. A weight of 0.26 g of catalyst was charged into the reactor tube and glass wool (Pyrex) was used to secure it in place. The reactor temperature was initially set to 250 C. prior to flowing chlorine at a rate of 5 cc/min. The beta-picoline feed rate was set to 0.13 mg/min (N2 flow 10 cc/min, chiller at 10 C.), while the reactor oven was ramped up to 350 C. over a one hour time period. At 350 C. the amount of beta-2-tet observed in the product gases was 65.6% (see Table 2).; Example 4; The catalyst, TOSOH HSZ-690 HOD (SAR 203) with the silica binder, was sized to a uniform particle size of 1-2 mm in diameter. A weight of 0.51 g of catalyst was charged into the reactor tube and glass wool (Pyrex) was used to secure it in place. The reactor temperature was initially set to 250 C. prior to flowing chlorine at a rate of 5 cc/min. The beta-picoline feed rate was set to 0.13 mg/min (chiller at 10 C.), with a nitrogen flow of 10 cc/min, while the reactor oven was ramped up to 350 C. over 2 hours. When the system had stabilized at 350 C. the amount of beta-2-tet observed in the product gases was 71.7% (see Table 2).; Example 5; The catalyst, TOSOH HSZ-690 HOD (SAR 203) with the silica binder, was sized to a uniform particle size of 1-2 mm. A weight of 0.51 g of catalyst was charged into the reactor tube and glass wool (Pyrex) was used to secure it in place. The reactor temperature was initially set to 250 C. prior to flowing chlorine at a rate of 5 cc/min. The beta-picoline feed rate was set to 0.25 mg/min (N2 at 10 cc/min, chiller at 20 C.), while the reactor oven was slowly ramped up to 350 C. over 2 hours. When the system had stabilized at 350 C. the amount of beta-2-tet observed in the product gases was 66.9% (see Table 2).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,108-99-6, its application will become more common.

Reference:
Patent; Campbell, Kent Douglas; Livingston, Dana Alan; Wan, Hawk Suewah; Larson, Kenneth Michael; Schoeman, Brian John; Lakso, Steven Roy; US2005/240024; (2005); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 108-99-6, 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 108-99-6, name is 3-Methylpyridine. This compound has unique chemical properties. The synthetic route is as follows.

The catalyst was prepared by the method as described in Example 3 and process conditions were maintained as per Example 5 except that the process was carried out at large scale. The catalyst was packed as per Example 5 in a tubular reactor. Total volume of the reactor was 75 liters and equipped with heating and cooling arrangement. The catalyst bed was heated in the presence of air/nitrogen to 250 C. beta-picoline, water and air were fed separately through a vaporizer from top of the reactor. The molar feed ratio of oxygen:water:beta-picoline was 20:40:1 and WHSV was 0.05 hr-1. The nicotinic acid was isolated by the method as described in Example 4. The vent gases and scrubbed liquid obtained from secondary absorber and mother liquor of first absorber was recycled back in the process with optimum purge. The nicotinic acid obtained was white colored. Selectivity: 90.8%; beta-picoline conversion of 94.6%. Assay: 99.58%.

According to the analysis of related databases, 108-99-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JUBILANT LIFE SCIENCES LTD; US2012/65405; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Adding a certain compound to certain chemical reactions, such as: 108-99-6, 3-Methylpyridine, 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, category: pyridine-derivatives, blongs to pyridine-derivatives compound. category: pyridine-derivatives

General procedure: In an oven dried glass tube containing a mixture of pyridine 1a (100 mg, 1.26 mmol), and potassium persulphate (683 mg, 2.53 mmol), formamide 2a (2 ml) was added and the reaction mixture was heated at 70 C. Upon the completion of the reaction (monitored by TLC), saturated sodium bicarbonate solution (5 mL) was added and the crude product was extracted in ethyl acetate (3 X 5 mL). The crude product was purified by column chromatography to furnish compound 3aa as a white crystalline solid (122 mg, 79% yield)

At the same time, in my other blogs, there are other synthetic methods of this type of compound,108-99-6, 3-Methylpyridine, and friends who are interested can also refer to it.

Reference:
Article; Mete, Trimbak B.; Singh, Ankit; Bhat, Ramakrishna G.; Tetrahedron Letters; vol. 58; 50; (2017); p. 4709 – 4712;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Related Products of 108-99-6, 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. 108-99-6, name is 3-Methylpyridine, molecular formula is C6H7N, 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: Catalyst (0.03 mmol), H2O (3 ml), substrate (4 mmol), and H2O2 (20 mmol, 30% aq.) were charged in the reaction flask, which was first bathed in cold water (about 283 K). The mixture was then stirred at room temperature for 16-24 h. The reaction was detected by thin-layer chromatography (TLC). After the reaction, the system was concentrated by evaporation, and the catalyst precipitated from the mixture after the addition of anhydrous ethyl alcohol. The recovered catalyst, obtained by filtration, was washed with anhydrous ethyl alcohol and diethyl ether and then used for the next oxidation after drying. The filtrate was extracted with dichloromethane. The combined organic layers were dried over anhydrous Na2SO4, and the pure products were obtained by evaporation or column chromatography. The products were analyzed by 1H NMR and 13C NMR.

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 108-99-6, 3-Methylpyridine.

Reference:
Article; Zhao, Wei; Wang, Xing; Yang, Chunxia; Synthetic Communications; vol. 44; 1; (2014); p. 150 – 160;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Electric Literature of 108-99-6, 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.

10 g of catalyst B was taken into a cylindrical fixed bed reactor with an inner diameter of 25 mm, and the plunger pump was pumped into a solution of 3-methylpyridine in carbon tetrachloride. The mass ratio of 3- methylpyridine to carbon tetrachloride was 1: The weight hourly space velocity of 10,3-methylpyridine is 6h, the chlorine gas flow rate is 2L/min, and the 3-methylpyridine and chlorine gas are vaporized by the preheating tube and then passed into the fixed bed reactor. The fixed bed reactor is used. The temperature was 400 C, the reaction was carried out for 4 h, the reaction product was passed through a condenser, and 2987 g of the reaction product mixture was obtained in a receiving tank. The ammonia solution was added to adjust to neutrality, and the pear-shaped funnel was separated to obtain an organic phase. 30 g of anhydrous sulfuric acid was added to the organic phase. Magnesium is dehydrated, suction filtered, and then rotary evaporated to remove carbon tetrachloride to give a pale yellow liquid. After analysis and detection, the product is a mixture of 2-chloro-5-trichloromethylpyridine, 2,3-dichloro-5-trichloromethylpyridine and 2,3,6-trichloropyridine, respectively. 77%, 16%, 7%. It is indicated that it is difficult to remove trichloromethyl group under the reaction conditions in the absence of water

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,108-99-6, its application will become more common.

Reference:
Patent; Chongqing Zhong Bang Technology Co., Ltd.; Xue Yi; Li Xueyong; Mu Dengyou; Chen Honglong; Qian Yong; (7 pag.)CN109734657; (2019); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem

Reference of 108-99-6, 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.108-99-6, name is 3-Methylpyridine, molecular formula is C6H7N, molecular weight is 93.13, as common compound, the synthetic route is as follows.

Example 7 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, 8.2 g of zinc sulfate were added into the solution and stirred for 30 minutes. Into the resultant solution were added 92.68 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 600C 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 40 to 60 nm. 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 1:30:70 (3-methylpyridine: oxygen: H2O) and where the bed temperature was controlled at 320C . The feed speed of 3-methylpyridine is 0.025 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 88.10%, a selectivity of nicotinic acid is 88.32%, and a selectivity of carbon dioxide is 9.25%.

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

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

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

108-99-6, 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. 108-99-6, name is 3-Methylpyridine, molecular formula is C6H7N, 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.

A 1000 mL four-neck bottle was placed in an ice water bath.Add 500g (content 99.5%,After the moisture content of 0.02%) 3-methylpyridine,Turn on the agitation,The dry hydrogen chloride gas (85g/h) is introduced under normal pressure.Water bath temperature control 0 C,Reacting in a dry anhydrous state,After all the white solid hydrochloride is formed,Stop stirring and continue to pass hydrogen chloride gas.The solid begins to dissolve,After introducing hydrogen chloride gas for 9 hours, 1265 g of liquid 3-methylpyridine hydrochloride was obtained (quantitative 3-methylpyridine content was39.53%).Transfer the above hydrochloride to a 2000 mL four-necked flask and place in an oil bath.After the stirring is started and the temperature is raised to 125 C, the chlorine gas after drying is started.Ventilation speed 50g/h,After 8h, the gas phase detection result was 3-methylpyridine: 3-chloromethylpyridine = 45:52 (gas phase qualitative ratio),Stop the chlorine and cool down to 110 C, at this temperature,Distilled under reduced pressure at a pressure of -0.08 MPa,A total of 236 g of distillate was obtained.Is unreacted 3-methylpyridine,The quantitative 3-methylpyridine content is 98.2%;The remaining bottom material is a light yellow solid.3-chloromethylpyridine hydrochloride,A total of 459.9g,The quantitative 3-chloromethylpyridine content is 73.88%,The yield was calculated to be 93.26%.

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. 108-99-6, 3-Methylpyridine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nanjing Hong Sun Biochemical Co., Ltd.; Nanjing Hong Sun Co., Ltd.; Zhan Xinhua; Zhong Jingsong; Wang Fujun; Chen Honglong; Mu Dengyou; Yang Cheng; (5 pag.)CN108409641; (2018); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem