Category: ethers-buliding-blocks

Application of 450-88-4, 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. 450-88-4, name is 1-Bromo-4-fluoro-2-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

Diisopropylamine (9.6 mL, 69 mmol) was dissolved in THF (100 mL) under nitrogen atmosphere. The solution was cooled to -78 C, and n-BuLi (21.6 mL, 2.5M in hexanes) was added over 10 mm. The resulting solution was stirred at -78 C for an additional 20 mm. Then, a solution of 1-bromo-4-fluoro-2-methoxybenzene (10 g, 49 mmol) in THF (20 mL) was added dropwise over 15 mm. The mixture was stirred at -78 C for 1 hour. DMF (4.2 mL, 54 mmol) was added dropwise over 5 mm, and the reaction mixture was stirred at -78 C for another 45 mm. Saturated aqueous NH4Cl (50 mL) was added, and the mixture was allowed to warm to room temperature and then diluted with Et20 (200 mL) and 2N HCl (100 mL). The organic layer was separated, and the aqueous layer was extracted with Et2O (2×50 mL). The combined organics were washed with brine (50 mL), dried (Na2SO4), concentrated in vacuo and purified by column chromatography on silica gel (1:50 EA/PE) to afford the title compound as a yellow solid (9.7 g). 1H NMR (400 MHz, CDCl3): oe 10.35 (s, 1H), 7.77-7.74 (m, 1H), 6.92-6.87 (m, 1H), 3.97 (s, 3H).

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-4-fluoro-2-methoxybenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SERAGON PHARMACEUTICALS, INC.; SMITH, Nicholas, D.; GOVEK, Steven, P.; KAHRAMAN, Mehmet; JULIEN, Jackaline, D.; NAGASAWA, Johnny, Y.; DOUGLAS, Karensa, L.; BONNEFOUS, Celine; LAI, Andiliy, G.; WO2013/142266; (2013); A1;,
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Adding a certain compound to certain chemical reactions, such as: 168971-68-4, name is 1-Bromo-2-fluoro-4-(trifluoromethoxy)benzene, 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 168971-68-4, Safety of 1-Bromo-2-fluoro-4-(trifluoromethoxy)benzene

Reference Example 1432-Fluoro-4-(trifluoromethoxy)aniline A mixture of 4-bromo-3-fluoro(trifluoromethoxy)benzene (6.6 g, 26 mmol), benzophenone imine (6.4 mL, 38 mmol), Pd2(dba)3 (0.58 g, 0.64 mmol), Xantphos (1.5 g, 2.6 mmol) and sodium tert-butoxide (3.7 g, 38 mmol) in 1,4-dioxane (120 mL) was stirred at 100 C. under N2 atmosphere for 5 h. After stirring at room temperature overnight, the mixture was concentrated under reduced pressure. The residue was partitioned between AcOEt and water. The organic layer was washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure. The residue was chromatographed on silica gel (0/100-5/95 AcOEt/hexane) to give a yellow oil. The residual oil was dissolved in THF (150 mL), and 1 M HCl aqueous solution (50 mL) was added to the mixture. After stirring at room temperature for 1 h, the mixture was basified with 8 M NaOH aqueous solution and extracted with diethyl ether. The organic layer was washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure. The residue was chromatographed on silica gel (0/100-5/95 AcOEt/hexane) to give the title compound (4.2 g, 85% yield) as a pale yellow oil: 1H NMR (300 MHz, DMSO-d6): delta ppm 5.36 (2H, s), 6.75-6.85 (1H, m), 6.89-6.94 (1H, m), 7.12 (1H, dd, J=11.7, 2.3 Hz).

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-Bromo-2-fluoro-4-(trifluoromethoxy)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Taniguchi, Takahiko; Kawada, Akira; Kondo, Mitsuyo; Quinn, John F.; Kunitomo, Jun; Yoshikawa, Masato; Fushimi, Makoto; US2010/197651; (2010); A1;,
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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. 10541-78-3, name is 2-Methoxy-N-methylaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 10541-78-3

Bromoacetyl chloride (0.425 mL, 5.1 mmol) in dry dichloromethane (5 mL) was added dropwise to a solution containing the respective amine (4.1 mmol) and a catalytic amount of dimethylaminopyridine (DMAP) (0.150 g, 30 mmol %) in dry dichloromethane (20 mL) maintained in an ice bath under argon atmosphere. The resulting solution was stirred at 0 C for 30 min, and the temperature was then increased to 25 C. After stirring for additional 4 hours, the reaction mixture was diluted with diethyl ether (50 mL). All of the stirring time was accomplished under an argon atmosphere. The organic layers were washed sequentially with a solution of 1 N HCl (2 ¡Á 50 mL), water (1 ¡Á 100 mL), saturated aqueous NaHCO3 (3 ¡Á 50 mL), and brine (5% w/v, 1 ¡Á 50 mL). Finally, the organic solution was dried over anhydrous MgSO4 and evaporated under vacuum, and the residue was purified by flash chromatography on silica gel and eluted with chloroform-methanol (40:1).

The synthetic route of 10541-78-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Giacobbo, Bruno Couto; Pissinate, Kenia; Rodrigues-Junior, Valnes; Villela, Anne Drumond; Grams, Estevao Silveira; Abbadi, Bruno Lopes; Subtil, Fernanda Teixeira; Sperotto, Nathalia; Trindade, Rogerio Valim; Back, Davi Fernando; Campos, Maria Martha; Basso, Luiz Augusto; Machado, Pablo; Santos, Diogenes Santiago; European Journal of Medicinal Chemistry; vol. 126; (2017); p. 491 – 501;,
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Reference of 162705-07-9, 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 162705-07-9 as follows.

General procedure: A solution of AmCA-4 (0.7mmol) in THF (5mL/mmol) was cooled at 0C and anhydrous pyridine (1.7mmol) and the corresponding phenyl chloroformate (1.0mmol) were added under inert atmosphere. The resulting mixture was stirred in the dark for 20minat 0C and for 1hat rt. After this time, H2O (3.4mL) and HCl 1M (1.7mL) were added to the reaction mixture, which was then extracted with CH2Cl2 (3¡Á20mL). The organic layer was washed with brine, and then dried on anhydrous Na2SO4. Removal of volatiles under reduced pressure afforded an oily residue which was subjected to column chromatography on silica-gel (Hexanes-EtOAc mixtures as eluant) obtaining the desired products with the yields indicated below. 6.1.2.1 53 Phenyl (Z)-(2-methoxy-5-(3,4,5-trimethoxystyryl)phenyl)carbamate (1) Off-white solid, m. p. 124-126C; 1H NMR (500MHz, CDCl3) delta 8.11 (br s, 1H), 7.52 (br s, 1H, NH), 7.39 (t, J?7.5Hz, 2H), 7.24 (t, J?7.5Hz, 1H), 7.19 (d, ?7.5Hz, 2H), 7.00 (d, J=8.5Hz, 1H), 6.76 (d, J=8.5Hz, 1H), 6.52 (s, 2H), 6.51 (d, J=12Hz, 1H), 6.45 (d, J=12Hz, 1H), 3.89 (s, 3H), 3.81 (s, 3H), 3.70 (s, 6H); 13C NMR (125MHz, CDCl3) delta (C) 152.9 (x 2), 151.3, 150.6, 146.9, 137.2, 132.7, 130.3, 126.9, (CH) 129.5, 129.3 (x 2), 129.2, 125.5, 123.9, 121.6 (x 2), 119.3, 109.6, 106.1 (x 2), (CH3) 60.8, 55.9 (x 2), 55.8; IR numax (cm-1) 3415 (N-H), 1750 (C=O); HR ESMS m/z 458.1588 [M+Na]+. Calc. for C25H25NNaO6, 458.1580.

According to the analysis of related databases, 162705-07-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Conesa-Milian, Laura; Falomir, Eva; Murga, Juan; Carda, Miguel; Meyen, Eef; Liekens, Sandra; Alberto Marco; European Journal of Medicinal Chemistry; vol. 147; (2018); p. 183 – 193;,
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Adding a certain compound to certain chemical reactions, such as: 53087-13-1, name is 1-(Benzyloxy)-3-bromobenzene, 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 53087-13-1, Safety of 1-(Benzyloxy)-3-bromobenzene

526 mg (2.0 mmol) of 1-(benzyloxy)-3-bromobenzene, 209 mul (2.4 mmol) of morpholine, 283 mg (2.8 mmol) of sodium t-butoxide, 9 mg (0.005 mmol) of tris(dibenzylidine acetone)dipalladium (O) 19 mg (0.015 mmol) of (No.)-BINAP were placed in a flask, 5 ml of toluene was added thereto, and the mixture was stirred at 80C for 20 hours. The reaction mixture was cooled to room temperature, 20 ml of ethyl acetate was added thereto, and filtered through Cellite. The resulting filtrate was concentrated under a reduced pressure, and the residue was subjected to column chromatography using 30% ethyl acetate/hexane as an eluent to obtain 430 mg (yield 80%) of 4- (3-(benzyloxy)phenyl)morpholine.

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-(Benzyloxy)-3-bromobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; KOREA RESEARCH INSTITUTE OF CHEMICAL TECHNOLOGY; OSCOTEC INC.; WO2005/123054; (2005); A1;,
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Application of 1663-61-2,Some common heterocyclic compound, 1663-61-2, name is (Triethoxymethyl)benzene, molecular formula is C13H20O3, 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.

General procedure: The orthoester (1.5 equiv) was added to a mixture of the 3-amino-2,2-dimethylpropionamide(1.0 equiv) in anhydrous ethanol (3 mL). Glacial acetic acid (2 equiv) was added and the reactionwas heated at reflux for 24 h. The reaction mixture was cooled and concentrated under vacuum.The product was hygroscopic and was best crystallized by adding purified chloroform and allowing itto sit under nitrogen for 4?7 days. Filtration and drying yielded the pure product.

The synthetic route of 1663-61-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gavin, Joshua T.; Annor-Gyamfi, Joel K.; Bunce, Richard A.; Molecules; vol. 23; 11; (2018);,
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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. 20781-20-8, name is (2,4-Dimethoxyphenyl)methanamine, A new synthetic method of this compound is introduced below., Quality Control of (2,4-Dimethoxyphenyl)methanamine

Added to the Schlenk reaction tube 18.1 mg (0.10 mmol) copper acetate, 16.0 mg (0.025 mmol) three (2, 2′ – bipyridyl) ruthenous, 16.0 mg (0.02 mmol) tert lithium ethoxide, using Schlenk double-row tube vacuum pumping, access oxygen state, adding 79 uL (0.5 mmol) 2, 4 – dimethoxybenzylamine, 2.5 ml dimethyl sulfoxide, the use of the Schlenk tube with double row sustained and the oxygen to the reaction system, the temperature control of the reaction system 35 C, white light LED lamp (wavelength 400 – 760 nm) irradiation, stirring for 20 hours after the, adding 3 ml saturated sodium acid sulfite aqueous solution and 10 ml ethyl acetate, extraction liquid, anhydrous magnesium sulfate drying, to remove the magnesium sulfate, the resulting organic phase is concentrated, the concentrate with silica gel column chromatography, to obtain 2, 4 – dimethoxy carbonitrile, yield 90%

The synthetic route of 20781-20-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; HUAIHAI INSTITUTE OF TECH; Huaihai Technology College; TAO CHUANZHOU; Tao Chuanzhou; WANG BIN; Wang Bin; SUN LEI; Sun Lei; LIU ZHOU; Liu Zhou; ZHAI YADONG; Zhai Yadong; (5 pag.)CN107814751; (2018); A;,
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Related Products of 35822-58-3, 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. 35822-58-3, name is 2-Bromobenzaldehyde diethyl acetal belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

As shown in Figure 2, 3.3 mmol of 2-bromobenzaldehyde diethanol and 3.8 mmol of nitrile ethyl acetate are mixed and diluted with ethyl acetate to 10 mL, and then the resulting solution is reacted by continuous flow at a flow rate of 1 mL / min The pump was pumped into the first HPLC column (containing 1g PS-perazine) and the second HPLC column (containing 1g PS-N-SO3) in sequence. At the same time, the first and second HPLC columns were immersed in a 50 C oil bath and reacted for 3 hours. . After the reaction was completed, the HPLC column was rinsed with ethyl acetate, the product was collected, ethyl acetate was evaporated, and recrystallized from ethanol to obtain a solid product with a yield of 89%.

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, 2-Bromobenzaldehyde diethyl acetal, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Huaqiao University; Xiong Xingquan; Liao Xu; (11 pag.)CN110818592; (2020); A;,
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Application of 450-88-4, A common heterocyclic compound, 450-88-4, name is 1-Bromo-4-fluoro-2-methoxybenzene, molecular formula is C7H6BrFO, 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.

Intermediate Example Int20.014-(4-bromo-3-methoxyphenoxy)-1-methylpiperidineTo a stirred suspension of sodium hydride (1.76 g; 60% w/w sodium hydride in oil) in DMF (55 mL) was added 1-methylpiperidin-4-ol (3.37 g) at 0 C. The mixture was stirred at r.t. for 30 min. 1-bromo-4-fluoro-2-methoxybenzene (3.0 g) was added and the mixture was stirred at 100 C for 1 h. Water was added and the mixture was extracted with ethyl acetate. The organic phase was washed with saturated sodium chloride solution, dried (sodium sulfate) and the solvent was removed in vacuum. Aminophase-silica-gel chromatography gave 3.65 g of the title compound.

The synthetic route of 450-88-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; SCHULZE, Volker; KOSEMUND, Dirk; WENGNER, Antje, Margret; SIEMEISTER, Gerhard; STOeCKIGT, Detlef; LIENAU, Philip; BRIEM, Hans; WO2012/160029; (2012); A1;,
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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. 34967-24-3, name is 3,5-Dimethoxybenzyl amine, A new synthetic method of this compound is introduced below., Formula: C9H13NO2

In a procedure analogous to Example 21, reaction of 3, 5-dimethoxybenzylamine and 2, [6-DICHIOROPYRAZINE FURNISHED THE PRODUCT (91%).] 1H-n. [M.] [R.] (CDCl3) [No.3. ]78 [(S,] 6H, OCH3), 4.49 (d, J= 5.4 Hz, [2H,] NCH2); 5. 12 (br [S,] [1H,] NH), [6.] 39 [(T,] J= 2. 1 Hz, 1H, ArH), 6.50 (d, J= 2.1 Hz, 2H, ArH), 7.75 (s, 1H, pyraz.- H), 7. [S2] [(S,] 1H pyraz.-H).

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; CYTOPIA PTY LTD; WO2003/99796; (2003); A1;,
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