Tag: M.W=100-200

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 1535-75-7 as follows. Quality Control of 2-(Trifluoromethoxy)aniline

General procedure: Acetamides (1a-1x, 1ab, 1ac and 1ba-1bc). To a solution of 2-phenylacetic acid (7.0mmol), 2-(trifluoromethoxy)aniline (7.7mmol) in anhydrous CH2Cl2 (25mL) were added EDCI (1.745g, 9.1mmol) and DMAP (256.6mg, 2.1mmol). The reaction mixture was stirred at room temperature overnight, diluted with HCl (1M) aqueous solution, and extracted with CH2Cl2 (3¡Á25mL). The combined organic phase was washed with saturated NaHCO3 aqueous solution and brine, dried over anhydrous Na2SO4, and concentrated under vacuum. Purification by flash chromatography (Silica gel, petroleum ether: ethyl acetate=50: 1 as eluent) gave the corresponding 2-phenyl-N-[2-(trifluoromethoxy)phenyl]acetamide compound.

According to the analysis of related databases, 1535-75-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhao, Xiao-Jing; Zhao, Jie; Sun, Xin; Liu, Ji-Kai; Wu, Bin; Tetrahedron; vol. 73; 25; (2017); p. 3463 – 3477;,
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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. 768-70-7, name is 3-Ethynylanisole, This compound has unique chemical properties. The synthetic route is as follows., name: 3-Ethynylanisole

General procedure: To a stirred solution of alkyne (12mmol, 1.2equiv) in 50mL DCM was added copper(I)-thiophene-2-carboxylate (CuTc, 95mg, 0.5mmol, 0.05equiv). The solution was cooled to 0C and treated dropwise with a solution of 10mmol sulfonyl azide in 10mL DCM. Then, the reaction mixture was stirred a further 12h, monitored by TLC. After reaction, it was diluted with 30mL saturated NH4Cl and extracted with DCM (30mL¡Á3). The combined organics were washed with brine, dried with Na2SO4 and concentrated in vacuo. The crude product was then purified by flash chromatography (Petroleum ether/EtOAc=5:1-1:1). Subsequent recrystallization from EtOAc/Petroleum ether provided the title triazoles substrates.

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 768-70-7.

Reference:
Article; Meng, Jiang; Ding, Xiangfeng; Yu, Xingxin; Deng, Wei-Ping; Tetrahedron; vol. 72; 1; (2016); p. 176 – 183;,
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Related Products of 51344-14-0, 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. 51344-14-0, name is N,N-Dimethyl-2-(p-tolyloxy)ethanamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

58.9 g (0.495 mol) of potassium bromide,Hydrogen peroxide 60 ml,Water 60 ml and 150 ml of chloroform were added to a liter of three bottles,Drop under ice bath32 ml concentrated sulfuric acid,Drop finished, remove the ice bath,Add 4- (2-dimethylaminoethoxy) toluene134 g (0.75 mol),The reaction solution was refluxed under light for 2 h,After completion of the reaction, the organic layer was separated, dried over anhydrous sodium sulfate, And the crude product was distilled under reduced pressure to give 185 g of a pale yellow liquid in a yield of 96%.

The synthetic route of N,N-Dimethyl-2-(p-tolyloxy)ethanamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Anhui Cheng Lian Pharmaceutical Technology Co., Ltd.; Liu Hui; (5 pag.)CN106748821; (2017); A;,
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Application of 52189-63-6, These common heterocyclic compound, 52189-63-6, name is 1-Fluoro-3,5-dimethoxybenzene, 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.

Weigh 1.5g of 1-fluoro-3,5-dimethoxybenzene and dissolve it with CH2Cl2.40 ml of BBr3/CH2Cl2 solution was added dropwise under ice bath, and reacted at room temperature overnight.After the end, the excess boron tribromide is quenched with methanol.Add ice water, stir, distill off most of the CH2Cl2 under reduced pressure, and extract the aqueous phase three times with ethyl acetate.The ethyl acetate layer was combined, dried with saturated brine, and EtOAc evaporated.The product was obtained in an amount of 1.2 g, which was used without further purification.

Statistics shows that 1-Fluoro-3,5-dimethoxybenzene is playing an increasingly important role. we look forward to future research findings about 52189-63-6.

Reference:
Patent; Cai Pei; Xiao Zuoqi; Ouyang Bo; Pan Tao; Zheng Yi; (7 pag.)CN109678915; (2019); A;,
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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. 33311-29-4, name is 4-(2-Methoxyethoxy)aniline, A new synthetic method of this compound is introduced below., Safety of 4-(2-Methoxyethoxy)aniline

4-(2-Methoxyethoxy)aniline (500mg) was added to acetic anhydride (2.38g) and the mixture was cooled down to 10C. HN03 (65% in water, 0.62ml) was added slowly in order to keep the temperature of the reaction mixture below 15C. After the end of the addition, the reaction mixture was allowed to warm to RT over 1 h, was quenched with ice-cold water and stirred for 10min. The resulting suspension was filtered off and dried in high vacuo. The resulting yellow powder was dissolved in dioxane (1.4ml) , treated with 6N HCl (1 .4ml_) and the reaction mixture was stirred at 70C for 3h. After cooling down to RT, water was added and the pH was adjusted to 10 with 1 M NaOH. The layers were separated and the aq. phase was extracted with EA. The combined org. layers were washed with brine, dried (Na2SO4) and evaporated in vacuo to afford 303mg of yellow solid. LC-MS (B): tR = 0.99min; [M+H]+: 213.05.

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; ACTELION PHARMACEUTICALS LTD; CAROFF, Eva; KELLER, Marcel; KIMMERLIN, Thierry; MEYER, Emmanuel; WO2013/114332; (2013); A1;,
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Adding a certain compound to certain chemical reactions, such as: 645-36-3, name is 2,2-Diethoxyethanamine, 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 645-36-3, Computed Properties of C6H15NO2

N-(3-Bromo-4-chlorobenzyl)-2,2-diethoxyethanamine To a solution of 3-bromo-4-chlorobenzaldehyde (10.0 g, 45 mmol) and 2,2-diethoxyethanamine (6.68 g,50 mmol) in 200 mL of DCM at RT, 0.5 mL of AcOH was added and the resulting mixture was stirred at RT for 30 min. To this mixture, NaCNBH3 (8.1 g, 135 mmol) was added in portions and then stirred at RT overnight. The reaction mixture was portioned between water and DCM. The organic layer was washed with water (80 mL x 2) and brine, dried over anhydrous Na2SO4, filtered and concentrated in vacuo to afford the desired product (11 g, 72% yield) as an oil. The crude product obtained was used directly in the next step without further purification

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

Reference:
Patent; ARAXES PHARMA LLC; LI, Liansheng; FENG, Jun; WU, Tao; REN, Pingda; LIU, Yi; LIU, Yuan; LONG, Yun, Oliver; WO2015/54572; (2015); A1;,
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Electric Literature of 1535-75-7, 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. 1535-75-7, name is 2-(Trifluoromethoxy)aniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Representative procedure for the 2-methyl-N,4-diphenylquinoline-3-carboxamide (Entry 22, Table 1): To the magnetically stirred solution of KOt-Bu (2 mmol) in THF (6 mL) at rt, was added methyl 2-methyl-4-phenylquinoline-3-carboxylate 3a (0.277 g, 1 mmol) followed by addition of aniline (0.093 mL, 1 mmol, 1 equiv) and the mixture was allow to stirred at rt until the completion of reaction (5 h, monitored by TLC) . After completion of reaction THF evaporated under rotary vacuum evaporation, crude reaction mixture was extracted with EtOAc (3 ¡Á 5 mL) and H2O (5 mL). The combined EtOAc extracts were dried (anh Na2SO4), filtered, and the filtrate was concentrated under rotary vacuum evaporation. The crude product was adsorbed on silica gel (230-400 mesh size, 500 mg), charged on to a flash chromatography column of silica-gel (230-400 mesh size, 2.5 g), and eluted with hexane-EtOAc (90:10) to obtain analytically pure 2-methyl-N,4-diphenylquinoline-3-carboxamide, 5a as white solid (0.219 g, 65%);

The synthetic route of 2-(Trifluoromethoxy)aniline has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tanwar, Babita; Kumar, Asim; Yogeeswari, Perumal; Sriram, Dharmarajan; Chakraborti, Asit K.; Bioorganic and Medicinal Chemistry Letters; vol. 26; 24; (2016); p. 5960 – 5966;,
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Application of 106877-20-7, 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. 106877-20-7, name is 3-Methoxy-4-(trifluoromethyl)aniline, This compound has unique chemical properties. The synthetic route is as follows.

step 3-; A 100 mL round bottom flask fitted with a stir bar and septum was charged with 84a (3.01) g and maintained nitrogen atmosphere. To the flask was added anhydrous dioxane (25 mL) and HOAc (7.5 mL). The solution was stirred rapidly in an ice bath and a solution of bromine and dioxane (20 mL, 0.135 g Br2/mL) was added dropwise over 30 min using a syringe pump. A beige precipitate formed and the mixture thickened. The ice bath was removed and the reaction mixture stirred at RT for 1 h. The reaction mixture was poured into a mixture of 1.0 M NaOH (150 mL) and 2.0 M Na2CO3 (150 mL) and extracted with DCM (3¡Á100 mL). The combined extracts were washed sequentially with 0.5 M Na2CO3 (150 mL) and brine (150 mL), dried (Na2SO4), filtered and concentrated in vacuo. The resulting pale yellow liquid slowly solidified and darkened to afford 84b (4.10 g) black crystalline solid.

The chemical industry reduces the impact on the environment during synthesis 3-Methoxy-4-(trifluoromethyl)aniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; de Vicente Fidalgo, Javier; Li, Jim; Schoenfeld, Ryan Craig; Talamas, Francisco Xavier; Taygerly, Joshua Paul Gergely; US2010/311760; (2010); A1;,
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944561-44-8, name is 2-[2-(2-Propynyloxy)ethoxy]ethylamine, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 944561-44-8

Example 3: Synthesis of XZ-14424 Compound 7 (107 mg), amine 17 (84 mg), and DIPEA (193 muL) in 5 mL DMF were stirred at 85 C for 16 hours. Water was added to the reaction mixture and extracted with EtOAc. The organic phase was washed with water x1, brine x1, dried over Na2SO4, filtered and evaporated to dryness. The resulting mixture was purified by column chromatography using EtOAc and hexanes as eluents to afford 50 mg compound 18 as a green solid. Yield 32%. 1H NMR (400 MHz, CDCl3) delta 7.98 (s, 1H), 7.62-7.35 (m, 1H), 7.11 (d, J = 7.1 Hz, 1H), 6.93 (d, J = 8.5 Hz, 1H), 4.92 (dd, J = 11.9, 5.3 Hz, 1H), 4.21 (d, J = 2.3 Hz, 2H), 3.78-3.66 (m, 6H), 3.49 (t, J = 5.4 Hz, 2H), 2.93- 2.68 (m, 3H), 2.48-2.41 (m, 1H), 2.18-2.09 (m, 1H) ppm.

The synthetic route of 944561-44-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOVENTURES, LLC; ZHENG, Guangrong; ZHOU, Daohong; ZHANG, Xuan; WANG, Yingying; CHANG, Jianhui; (269 pag.)WO2017/184995; (2017); A1;,
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Related Products of 6346-09-4, The chemical industry reduces the impact on the environment during synthesis 6346-09-4, name is 4,4-Diethoxybutan-1-amine, I believe this compound will play a more active role in future production and life.

3-(4,4-Diethoxy)-1,1-dimethylurea (IId). N,N-Dimethylcarbamoyl chloride (2.5 g) was added dropwise with cooling (5-7C) under argon to a solution of 3.74 g of 4,4-diethoxy-1-butanamine and4.77 g of triethylamine in 27 mL of benzene. The reaction mixture was stirred under cooling for 2 h. Then the precipitate was filtered off, the filtrate was evaporated in vacuum.

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, 4,4-Diethoxybutan-1-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Smolobochkin; Gazizov; Burilov; Pudovik; Russian Journal of General Chemistry; vol. 85; 7; (2015); p. 1779 – 1782; Zh. Obshch. Khim.; vol. 85; 7; (2015); p. 1217 – 1220,4;,
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