Category: 321-28-8

Electric Literature of 321-28-8, 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. 321-28-8, name is 1-Fluoro-2-methoxybenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Synthesis of 3-fluoro-4-methoxybromobenzene Into a flask of 5 l were charged 384 g (3.04 mol) of 2-fluoroanisole and 2.5 l of chloroform, to which was added dropwise 504 g (3.16 mol) of bromine over about 3 hours while cooling on an ice water bath at 10 C. The resulting mixture was stirred at room temperature over a night and heated under reflux for 8 hours. After the air cooling, the product was added with 1 l of water and 50 g of sodium bisulfite and sufficiently shaken to separate into two layers. The resulting organic layer was washed with an aqueous solution of 5% sodium hydrogen carbonate and further with 1 l of water and dried on magnesium sulfate. After magnesium sulfate was filtered off, the filtrate was concentrated and distilled under a reduced pressure (4 mmHg, bp: 93-96 C.) to obtain 585 g (yield: 94%) of 3-fluoro-4-methoxybromobenzene.

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, 1-Fluoro-2-methoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nippon Mining Co., Ltd.; US5098602; (1992); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 321-28-8, A common heterocyclic compound, 321-28-8, name is 1-Fluoro-2-methoxybenzene, molecular formula is C7H7FO, 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.

Under ice bath conditions,6.38 g (48 mmol) of aluminum trichloride and 40 mlDichloromethane is put into a 100ml round bottom flask, stirred and dissolved4.68 g (60 mmol) of acetyl chloride, maintaining the temperature at 5 to 10 C., stirring at 5 C. for 10 minutes, followed by dropwise addition of 2-fluoroanisole 5.04 g(40 mmol). The mixture is stirred at 5C for 1 hour and then poured into 100 ml of ice-water. The aqueous layer is extracted with dichloromethane (2 x 30 ml). The combined organic phases are washed with water (2 x 30 ml), dried over anhydrous magnesium sulphate, filtered, and petroleum ether is used. The product was recrystallized from ethyl acetate in 92.4% yield.

The synthetic route of 321-28-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Northeast Agricultural University; Zhang Xiuying; Yang Hongliang; (11 pag.)CN107686465; (2018); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Some common heterocyclic compound, 321-28-8, name is 1-Fluoro-2-methoxybenzene, molecular formula is C7H7FO, 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. Quality Control of 1-Fluoro-2-methoxybenzene

The crude product (1.0 g, 7.9 mmol) was dissolved in acetonitrile (15 mL) and N-bromosuccinimide (1.4 g, 8.7 mmol) was added and reacted at 70 C for 3 h. After the reaction was completed, most of the acetonitrile was distilled off, 30 mL of water was added, the mixture was stirred for 10 min and extracted with ethyl acetate (3 × 20 mL). The combined organic phases were dried over anhydrous magnesium sulfate and separated by column chromatography (pure petroleum ether as eluent) The brominated product (intermediate A_2c) was obtained as a light yellow oily liquid (1.4 g, yield 86%) oA-2c: SH (300 MHz; CDCl 3) 7.23-7.16 (2H, m), 6.82 (D, J = 8.7Hz), 3.86 (3H, s); delta (75MuEtazeta; CDC13) 152.3 (d, Jc, F = 249.0Hz), 147.1 (d, 119.6 (d, J = 21.1 Hz), 114.6 (d, J = 2.2 Hz), 111.9 (d, J = 8.2 Hz), 56.4

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 321-28-8, its application will become more common.

Reference:
Patent; Chinese Academy Of Sciences Chemical Institute; Yu Chuyi; Li Yixian; Jia Tengdun; Zhao Xuan; (27 pag.)CN104557654; (2017); B;,
Ether – Wikipedia,
Ether | (C2H5)2O – 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. 321-28-8, name is 1-Fluoro-2-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 321-28-8

A solution of 2-fluoro-anisole (6.0 g, 47 mmol) and N, N, Nu’, ‘- tetramethylethylenediamine in THF (250 mL) was cooled to – 78 C and treated dropwise with sec -butyl lithium (1.3 M in cyclohexane, 38 mL, 49 mmol). The mixture was stirred for 2 h at – 78 C and then treated with dimethylformamide (3.6 mL, 47 mmol). Stirring continued for an additional 10 min and then acetic acid (20 mL) followed by water (150 mL) was added to the mixture. The mixture was warmed to ambient temperature and then diluted with ethyl acetate. The organic layer was washed with 1 M HCI, and brine. The organic layer was dried over Na2S04 and concentrated under reduced pressure to give crude 2-flouro-3-methoxybenzaldehyde (4.7 g, yield 64%) as a yellow solid. NMR (400 MHz, CDC13) (ppm) 10.40 (s, 1H), 7.45-7.40 (m, 1H), 7.23-7.18 (m, 2H), 3.94 (s, 3H).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 321-28-8.

Reference:
Patent; ANACOR PHARMACEUTICALS, INC.; AKAMA, Tsutomu; JARNAGIN, Kurt; ZHANG, Yong-kang; ZHOU, Yasheen; PLATTNER, Jacob, J.; SULLIVAN, David, C.; WO2015/13318; (2015); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 321-28-8, name is 1-Fluoro-2-methoxybenzene, belongs to ethers-buliding-blocks compound, 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 321-28-8, name: 1-Fluoro-2-methoxybenzene

A stirred solution of 2-fluoroanisole (33.7 mL, 301 MMOL) in chloroform (250 mL) was cooled to 0C and treated drop-wise with chlorosulfonic acid (50.0 mL, 752 MMOL). After stirring at room temperature for 14 hours, the reaction mixture was poured into ice-water (700 mL) and the separated, aqueous phase extracted with chloroform (2 x 200 mL). The combined organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated IN VACUO TO YIELD 3-FLUORO-4- METHOXYBENZENESULFONYL CHLORIDE as a fine, white solid (58.6 g, 87%), m. p. 80C ; 1H NMR (400 MHz, DMSO-d6) 5 : 7.32 (m, 1H), 7.25 (dd, J= 11.5, 2.0 Hz, 1H), 7.05 (t, J = 8. 5 HZ, 1 H), 3.78 (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.

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. 321-28-8, name is 1-Fluoro-2-methoxybenzene, A new synthetic method of this compound is introduced below., Quality Control of 1-Fluoro-2-methoxybenzene

General procedure: An oven-dried 20 mL scintillation vial, equipped with a magnetic stir-bar, was charged with the starting material (1.0 equiv), DDQ (1.0 equiv), trifluoromethanesulfonic acid (1.4% v/v, 3.0 equiv), and 1,2-dichloroethane (0.05 M). The reaction mixture was then allowed to stir at ambient temperature for 10 h. After this time, methanol (0.05M) was added, and the solution was then allowed to stir at ambient temperature for an additional hour. Upon addition of the methanol, some solids precipitated out of the solution. Then, the solvent was removed from the heterogeneous mixture under reduced pressure. The crude material was purified by either recrystallization (methanol/DCM) or silica-gel column chromatography (hexanes/DCM) to give the title compounds.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference of 321-28-8, These common heterocyclic compound, 321-28-8, name is 1-Fluoro-2-methoxybenzene, 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.

Step 1 Preparation of 3′-fluoro-4′-methoxy-acetophenone Acetyl chloride (51.0 g, 0.65 mol) was added dropwise to a stirred solution of aluminum chloride (80.0 g, 0.6 mol) and chloroform (750 mL), maintaining the temperature between 5-10 C. The mixture was stirred for 10 minutes at 5 C. before the dropwise addition of 2-fluoroanisole (62.6 g, 0.5 mol). The mixture was stirred at 0-10 C. for 1 hour and poured into ice (1 L). The resultant layers were separated and the aqueous layer was extracted with dichloromethane (2*250 mL). The combined organic layers were washed with water (2*150 mL), dried over anhydrous MgSO4, filtered and concentrated in vacuo to a volume of 300 mL. Hexanes were added and a white solid formed which was isolated by filtration and air dried. This material was recrystallized from a mixture of dichloromethane and hexanes to afford (77.2 g, 92%) of material suitable for use in the next step: mp 92-94 C.

The synthetic route of 321-28-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; G. D. Searle & Co.; US6136839; (2000); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – 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 321-28-8 as follows. Quality Control of 1-Fluoro-2-methoxybenzene

1-Fluoro-2-methoxybenzene a13 (0.0126 g, 0.10 mmol), acridine photosensitizer (A) (0.0029 g, 0.005 mmol) and L-valine ethyl ester b1 were added sequentially under argon protection. 0.0218 g, 0.15 mmol), 1,2-dichloroethane (DCE) 2.0 mL.The reaction was irradiated for 48 hours under a 6W blue light at room temperature.After completion of the reaction, the solvent was evaporated under reduced pressure and purified by column chromatography, eluting solvent: (V) petroleum ether / (V) ethyl acetate = 20/1.A yellow liquid (30) (0.0188 g, 95%) was obtained.

According to the analysis of related databases, 321-28-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Central China Normal University; Zhou Shaolin; Shi Weimin; (27 pag.)CN110294685; (2019); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 321-28-8, name is 1-Fluoro-2-methoxybenzene, belongs to ethers-buliding-blocks compound, 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 321-28-8, Recommanded Product: 321-28-8

Step 1: Preparation of 3′-fluoro-4′-methoxy-acetophenone. Acetyl chloride (51.0 g, 0.65 mol) was added dropwise to a stirred solution of aluminum chloride (80.0 g, 0.6 mol) and chloroform (750 mL), maintaining the temperature between 5-10 C. The mixture was stirred for 10 minutes at 5 C before the dropwise addition of 2-fluoroanisole (62.6 g, 0.5 mol). The mixture was stirred at 0-10 C. for 1 hour and poured into ice (1 L). The resultant layers were separated and the aqueous layer was extracted with dichloromethane (2*250 mL). The combined organic layers were washed with water (2*150 mL), dried over anhydrous MgSO4, filtered and concentrated in vacuo to a volume of 300 mL. Hexanes were added and a white solid formed which was isolated by filtration and air dried. This material was recrystallized from a mixture of dichloromethane and hexanes to afford material suitable for use in the next step (77.2 g, 92%): mp 92-94 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.

Reference:
Patent; G.D. Searle & Co.; US6407140; (2002); B1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

These common heterocyclic compound, 321-28-8, name is 1-Fluoro-2-methoxybenzene, 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. Recommanded Product: 1-Fluoro-2-methoxybenzene

Step 1. Preparation of 1-(3-fluoro-4-methoxyphenyl)-2-phenyl-ethan-1-one. Aluminum chloride (42.17 g, 316 mmol) and dichloromethane (350 mL) were cooled to 2 C. and phenylacetylchloride (40.50 g, 262 mmol) in dichloromethane (30 mL) was added. 2-Fluoroanisole (32.77 g, 260 mmol) in dichloromethane (30 mL) was added. The cooling bath was removed, and the mixture was stirred for 1 hour. The reaction mixture was poured into concentrated HCl (150 mL), filtered through diatomaceous earth, washed with saturated aqueous NaHCO3, dried over MgSO4, and concentrated. A white solid was obtained by crystallization from dichloromethane/hexane (29.2 g, 46%): mp 105-106 C.

The synthetic route of 1-Fluoro-2-methoxybenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; G. D. Searle & Co.; US5859257; (1999); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem