Category: 450-91-9

Adding a certain compound to certain chemical reactions, such as: 450-91-9, name is 4-Fluoro-2-methoxyaniline, 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 450-91-9, Recommanded Product: 450-91-9

4-Fluoro-2-methoxyaniline (2.4 g, 17.00 mmol)Was added portionwise to concentrated H2SO4 (15 mL) cooled in an ice / water bath,The temperature was maintained below 15 & lt; 0 & gt; C during the addition.The mixture was stirred until all of the formed solids had dissolved.KNO3 (0.815 mL, 17.00 mmol) was added in portions,So as to keep the temperature below 10 C. The mixture was stirred overnight and then poured onto ice / water.The mixture was basified with concentrated NH4OH. The resulting solid was filtered off,Then dissolved in CH2Cl2, washed with water, dried (Na2SO4),Concentrated on silica gel. Using FCC for purification,Eluting with 50% by weight of heptane in CH2Cl2,The title compound was obtained as a yellow crystalline solid (2.450 g, 77%).

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

Application of 450-91-9, These common heterocyclic compound, 450-91-9, name is 4-Fluoro-2-methoxyaniline, 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 b: Compound 1a2 (8.0 g, 43 mmol) was added into a 500 ml reaction flask, and concentrated sulfuric acid (100 ml) was added to dissolve the substrate under constant agitation. At -20 C., concentrated nitric acid (6.15 ml, 48 mmol) was slowly added dropwise with stirring, and the reaction mixture was stirred for 5 mins at this temperature. The reaction progress was monitored by TLC. After completion of the reaction, the mixture was poured into ice water. Sodium hydroxide/water solution (150 ml/300 ml) were added slowly to the reaction system at -20 C. in an ice-water bath, and the mixture was adjusted to pH 8-9. The reaction solution was extracted with EA/water system for three times, the organic layer was separated, washed with water, saturated brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure to give compound 1a (8.7 g) which was used directly in the next reaction. Yield: 80%; purity: 100%; MS m/z (ESI): 187.0 [M+H]+; 1H NMR (400 MHz, DMSO-d6): delta 7.34 (d, J=7.8 Hz, 1H), 7.04 (d, J=13.4 Hz, 1H), 5.25 (brs, 2H), 3.90 (s, 3H).

Statistics shows that 4-Fluoro-2-methoxyaniline is playing an increasingly important role. we look forward to future research findings about 450-91-9.

These common heterocyclic compound, 450-91-9, name is 4-Fluoro-2-methoxyaniline, 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: 4-Fluoro-2-methoxyaniline

39g material take B1-2, concentrated sulfuric acid was added to 500ml was added under ice-salt bath. Controlling the temperature of the whole solution was stirred below 10C. was added maintaining the temperature below 10C, 1ep potassium nitrate, was stirred overnight at room temperature. The next day, poured into ice water, adjusted with ammonia PH>7, extracted with ethyl acetate, dried and purified through column chromatography to give 44g product.

The synthetic route of 4-Fluoro-2-methoxyaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang Tongyuankang Pharmaceutical Co., Ltd.; Wu Yusheng; Geng Yang; Meng Qingguo; Niu Chengshan; Liang Apeng; (18 pag.)CN108558835; (2018); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Application of 450-91-9, These common heterocyclic compound, 450-91-9, name is 4-Fluoro-2-methoxyaniline, 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.

To a mixture of 4-fluoro-2-methoxyaniline (25.0 g, 177 mmol), K2C03 (36.7 g, 266 mmol) and Nal (10.6 g, 0.07 mmol) in /- PrOH (250 ml.) was added bis(2-chloroethyl)amine hydrochloride (47 g, 177 mmol). The reaction mixture was refluxed overnight. The solvent was removed and the residue was purified by column chromatography (petroleum ether/EtOAc = 10:1 ) to provide 1 -(4-fluoro-2-methoxyphenyl)piperazine. MS: m/z 212.36 [M+H] +.

The synthetic route of 450-91-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KEZAR LIFE SCIENCES; JOHNSON, Henry; (166 pag.)WO2019/178510; (2019); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – 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. 450-91-9, name is 4-Fluoro-2-methoxyaniline, A new synthetic method of this compound is introduced below., Product Details of 450-91-9

The compound 2-a-2 (8.0g, 43mmol) in 500mL reaction flask, under stirring concentrated sulfuric acid was added (100 mL) to dissolve the substrate. At -20 deg. C condition, to the stirred reaction flask was slowly added dropwise concentrated nitric acid (6.15 mL, 48mmol), and held at that temperature for 5 minutes. The progress of the reaction by TLC, until complete reaction of the substrate, poured into ice water. -20 deg. C kept ice bath, was slowly added to the reaction system sodium hydroxide / water solution (150mL / 300 mL), adjusted to pH 8-9. After completion of the reaction solution with ethyl acetate / water system was extracted three times, the organic layer was separated, washed with water, saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give 4-fluoro-2-methoxy -5-nitroaniline compound 2-a-3 (8.7g), was used directly in the next reaction. Yield: 80%; purity: 100%;

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:
Patent; Shanghai Haiyan Pharmaceutical Technology Co. Ltd; Yangtze River Pharmaceutical Group Co., Ltd; Jin, Yunzhou; Bo, Ping; He, Qi; Lan, Jiong; Zhou, Fusheng; Zhang, Liang; He, Xiangyu; (59 pag.)CN105524068; (2016); A;,
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. 450-91-9, name is 4-Fluoro-2-methoxyaniline, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 450-91-9

A solution of 4-fluoro-2-(methyloxy)aniline (Heterocycles 1992, 34, 2301-2311) (5.6 g, 40 mmol) and triethylamine (6.9 ml, 50 mmol) in dichloromethane (200 ml) at 0¡ãC was treated with acetyl chloride (2.85 ml, 40 mmol). After stirring at room temperature for 1 hour the solution was washed with 2N hydrochloric acid. The organic phase was separated, washed with water and brine then dried over anhydrous magnesium sulfate and concentrated in vacua. The residue was purified by chromatography on silica gel (1:5 to 1:2 ethyl acetate in dichloromethane) to affordthe title compound. MS (ES+) m/e 184 [M+H]+.

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 450-91-9.

Reference:
Patent; GLAXO GROUP LIMITED; WO2006/10629; (2006); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Synthetic Route of 450-91-9, 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 450-91-9 as follows.

Under an ice bath condition, 4-fluoro-2-methoxyaniline (Intermediate 102) (15 g, 106.4 mmol, 1.0 eq) was added dropwise to a concentrated sulfuric acid (150 mL) while controlling the temperature around 0C during the course of addition. After the forming solid was dissolved completely, potassium nitrate (11 g, 106.4 mmol, 1.0 eq) was added portionwise and the reaction was continued for 1 hour under this condition. The reaction was poured into ice water and the pH was adjusted to basic by sodium hydroxide. A vast amount of solid was precipitated out which was filtered and washed with water, petroleum ether, dried in air to give 4-fluoro-2-methoxy-5-nitroaniline as a brown solid (18 g, yield: 77%). LCMS (ESI): m/z 187 [M + H]+.

According to the analysis of related databases, 450-91-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Guangzhou Bebetter Medicine Technology Co., Ltd.; CAI, Xiong; QIAN, Changgeng; WENG, Yunwo; LIU, Bin; WANG, Yanyan; LIN, Mingsheng; LI, Junqi; QING, Yuanhui; YOU, Huajin; ZHOU, Shiqing; XUE, Weicai; (76 pag.)EP3345900; (2018); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – 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. 450-91-9, name is 4-Fluoro-2-methoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 450-91-9

Step 1: 2-bromo-4-fluoro-6-methoxyaniline To a solution of 4-fluoro-2-methoxyaniline (14.4 g, 0.1 mol) in 300 mL of dry DMF was added NBS (17.8 g, 0.1 mol) in small portions at 0-5¡ã C. under nitrogen, then the resulting mixture was stirred at room temperature overnight. The mixture was diluted with water, extracted with ethyl acetate. The combined organic layers were washed with water, brine, dried over sodium sulfate, filtered and concentrated under reduced pressure to give 2-bromo-4-fluoro-6-methoxyaniline (28 g crude).

The synthetic route of 450-91-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Arrington, Kenneth L.; Burgey, Christopher; Gilfillan, Robert; Han, Yongxin; Patel, Mehul; Li, Chun Sing; Li, Yaozong; Luo, Yunfu; Lei, Zhiyu; US2014/100231; (2014); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem