Month: June 2021

Related Products of 2752-17-2, 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. 2752-17-2, name is 2,2′-Oxydiethanamine, This compound has unique chemical properties. The synthetic route is as follows.

1-Hydroxypyrene-2-carbaldehyde 3 (100 mg, 0.41 mmol) wasdissolved in CH2Cl2 and 2,2′-oxybis (ethylamine) (0.02 mL,0.20 mmol) was added to the reaction mixture. The reactionmixture was stirred at RT for 12 h. The precipitate formed wasfiltered and washed with cold CH2Cl2 to give 2 as a yellow solid(176 mg, 76.6%). m.p. 200 C. 1H NMR (CDCl3, 250 MHz): delta 14.53(s, OH), 8.61 (s, 2H), 8.32 (d, J 9.10 Hz, 2H), 7.99-7.80 (m, 8H), 7.54(s, 2H), 7.35 (d, J 8.98 Hz, 2H), 3.91 (s, 8H). 13C NMR (CDCl3,62.5 MHz): delta 167.16, 156.66, 132.52, 132.18, 127.00, 127.12, 126.88,126.81, 126.66, 125.97, 124.77, 124.20, 123.90, 122.96, 121.49, 119.52,115.34, 69.91, 58.44, 30.92. HRMS (FAB) calcd for C38H29N2O3[M + H]+ 561.2100; found 561.2178.

The chemical industry reduces the impact on the environment during synthesis 2,2′-Oxydiethanamine. I believe this compound will play a more active role in future production and life.

Reference:
Article; Hu, Ying; Liu, Yifan; Kim, Gyoungmi; Jun, Eun Jin; Swamy; Kim, Youngmee; Kim, Sung-Jin; Yoon, Juyoung; Dyes and Pigments; vol. 113; (2015); p. 372 – 377;,
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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

Into a vial was added the 4-bromo-2-fluoro-N-thiazol-2-yl-benzenesulfonamide (2.60 g, 0.00771 mol), sodium tert-butoxide (1.78 g, 0.0185 mol), 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene (0.27 g, 0.00046 mol), tris(dibenzylideneacetone)dipalladium(0) (0.14 g, 0.00015 mol) and 1,4-dioxane (24.1 mL, 0.308 mol). Argon was bubbled for 15 minutes. 2,4-Dimethoxybenzylamine (1.40 mL, 0.00925 mol) was added and the reaction mixture was heated at 100 C. overnight. The reaction mixture was cooled to room temperature then filtered over Celite. The filtrate was concentrated to give the crude product that was purified via automated flash chromatography (silica gel, 50% EtOAc in hexanes to 100% EtOAc) to give the product as a yellow solid (2.59 g, 79.3%)

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; Icagen; US2009/23740; (2009); A1;,
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Some common heterocyclic compound, 645-36-3, name is 2,2-Diethoxyethanamine, molecular formula is C6H15NO2, 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. HPLC of Formula: C6H15NO2

[00114] To a glass reactor was charged 3,5-dichlorobenzaldehyde. Absolute ethanol was added to the batch slowly (this addition is mildly exothermic) and agitation started. 2,2- Diethoxyethylamine (1.03 equiv) was slowly added to the batch, keeping the batch temperature at 20-78 C. The batch was then heated to 76-78 C for 2 h. GC-MS analysis indicated reactioncompletion (starting material < 1%). The batch was cooled to ambient temperature for work-up. The batch was concentrated in vacuo to a residue and azeotroped with heptanes (x2). The residue was cooled and held at 0-5 C for 12 h to form a suspension. The solids were collected by filtration and the cake was washed with cold (0-5 C) heptanes, and dried under hot nitrogen (45-5 0 C) to afford Compound 2? as a white solid (94% yield). These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 645-36-3, its application will become more common. Reference:
Patent; SARCODE BIOSCIENCE INC.; ZELLER, James, Robert; VENKATRAMAN, Sripathy; BROT, Elisabeth, C.A.; IYER, Subashree; HALL, Michael; WO2014/18748; (2014); A1;,
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Synthetic Route of 2688-84-8, 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. 2688-84-8, name is 2-Phenoxyaniline, This compound has unique chemical properties. The synthetic route is as follows.

5.58.1 3-(2-Phenoxyphenylamino)phthalic acid dimethyl ester A mixture of 3-iodophthalic acid dimethyl ester (1.0 g, 3.1 mmol), 2-phenoxyaniline (0.57 g, 3.1 mmol), Pd2(dba)3 (0.13 g, 0.14 mmol), rac-BINAP (0.058 g, 0.093 mmol), and cesium carbonate (1.4 g, 4.3 mmol), in 6 mL toluene was heated to reflux under nitrogen for 24 hours. The reaction mixture was cooled, diluted with CH2Cl2 (10 mL), and filtered through Celite, and the filter was washed with additional CH2Cl2 (30 mL). The filtrate was evaporated, and the residue was chromatographed using a hexanes-ethyl acetate gradient, eluting 0.86 g of the product at 80:20 hexanes-ethyl acetate, in 73% yield: 1H NMR (CDCl3) delta 3.75 (s, 3H), 3.86 (s, 3H), 6.93-7.03 (m, 4H), 7.06-7.12 (m, 2H), 7.17 (dd, J=7.3 Hz, J=1.0 Hz, 1H), 7.29-7.38 (m, 4H), 7.46 (d, J=8.4 Hz, 1H), 7.89 (s, 1H).

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

Reference:
Patent; Muller, George W.; Chen, Roger Shen-Chu; Man, Hon-Wah; Ruchelman, Alexander L.; US2007/49618; (2007); A1;,
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Related Products of 2752-17-2, 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 2752-17-2 as follows.

Compounds 1 and 2 were prepared by the following procedure: 2-(4-chloro-3-nitrophenyl)-2-oxoethyl 2-aminobenzoate or 2-(4-amino-3-nitrophenyl)-2-oxoethyl 2-aminobenzoate (44.8 mmol) was suspended in polyphosphoric acid (167.3 g). The reaction mixture was heated to 100 C and stirred for 90 min. The mixture was then poured into H2O/crushed ice (700 ml). The precipitated product was filtered, washed with H2O, dried and recrystallized from 2-methoxyethanol. Compounds 3-17 were prepared by the following general procedure: quinolinone 1 (200 mg, 0.63 mmol) was added to a solution of amine (6.3 mmol) and N-methylpyrrolidone (1.0 ml) and the mixture was stirred at 110 C for 2 h. After cooling to room temperature, H2O (20 ml) was added and the pH adjusted to 7 with dilute HCl (1:3). The precipitated solid was collected by suction, washed thoroughly with H2O and dried at 80 C. The crude product was recrystallized from 2-methoxyethanol.

According to the analysis of related databases, 2752-17-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Motyka, Kamil; Hlava?, Jan; Soural, Miroslav; Hradil, Pavel; Krej?i, Petr; Kvapil, Lubomir; Weiss, Milo?; Tetrahedron Letters; vol. 52; 6; (2011); p. 715 – 717;,
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Synthetic Route of 5414-19-7, 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. 5414-19-7, name is 1-Bromo-2-(2-bromoethoxy)ethane belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of 3-amino-l-brotaunoisoquinoline (444 mg, 2.00 mmol) in anhydrous dimethylformamide (10175 mL) was added sodium hydride (60%, unwashed, 96 mg, 2.4 mmol) in one portion. The mixture was stirred at 25 0C for 5 min before 2-bromoethyl ether (90%, 250 DL, 2.00 mmol) was added. The mixture was stirred at 25 0C for 5 h and at 75 0C for 72 h before it was cooled to 25 0C, quenched with saturated ammonium chloride solution and diluted with ethyl acetate. The organic layer was separated, washed with water and brine, dried with Na2SO4, filtered and concentrated. Purification of the residue on silica gel eluting with 0% to 70% ethyl acetate/hexanes afforded Cap-143, step a as a yellow solid (180 mg, 31%) . Rt = 1.75 min (Cond. -MS-Wl) ; 90% homogenity index; LCMS: Anal. CaIc. for [M+H] + C13H14BrN2O: 293.03; found: 293.04.

The synthetic route of 1-Bromo-2-(2-bromoethoxy)ethane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; LAVOIE, Rico; BENDER, John A.; BACHAND, Carol; RUEDIGER, Edward H.; KADOW, John F.; WO2010/120621; (2010); A1;,
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Application of 93919-56-3,Some common heterocyclic compound, 93919-56-3, name is (4-(Trifluoromethoxy)phenyl)methanamine, molecular formula is C8H8F3NO, 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.

[000214] To a stirred solution of 6 (40 mg, 0.14 mmol) in DMF (3 mL) under argon atmosphere was added CDI (71.7 mg, 0.17 mmol) at 0 C; warmed to RT and stirred for 2 h. To this were added (4-(trifluoromethoxy) phenyl) methanamine 172 (33.8 mg, 0.17 mmol), and diisopropyl ethyl amine (0.05 mL, 0.29 mmol) and stirred for 16 h. The reaction was monitored by TLC; after completion of the reaction, the reaction mass was diluted with water (15 mL) and stirred for 1 h. The precipitate was filtered or extracted with EtOAc or CH2C12 and the obtained solid was dried in vacuo or purified by column chromatography or triturated to afford the desired product.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route (4-(Trifluoromethoxy)phenyl)methanamine, its application will become more common.

Reference:
Patent; INDIANA UNIVERSITY RESEARCH AND TECHNOLOGY CORPORATION; ASSEMBLY BIOSCIENCES, INC.; TURNER, William W.; ARNOLD, Lee Daniel; MAAG, Hans; ZLOTNICK, Adam; WO2015/138895; (2015); A1;,
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Application of 1535-73-5,Some common heterocyclic compound, 1535-73-5, name is 3-Trifluoromethoxyaniline, molecular formula is C7H6F3NO, 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. Preparation of Additional N-(3-oxo-2-(optionally substituted phenyl)isoindolin-4-yl) carboxamides of the Invention: Synthesis of 7-nitw-2-(3-(trifluowmethoxy)phenyl)isoindolin-l-one (6):A mixture of methyl 2-(bromomethyl)-6-nitrobenzoate from Example 1, Step 2 (3; 0.86 g, 3.14 mmol), 3-(trifluoromethoxyl)benzenamine (21; 0.56 g, 3.14 mmol) and HOAc (0.3 mL) in dioxane (3 mL) was stirred in microwave at 140 0C for 20 min. The mixture was adjust to pH=7 and extracted with ethyl acetate (3 x 25 mL). The combined organic layers were dried over Na2SO4, concentrated in vacuo and purified by chromatography on silica gel to afford 7-nitro-2-(3- (trifluoromethoxy)phenyl)isoindolin-l-one 6 (0.67 g, 1.98 mmol, 63percent). MS (ESI) calcd for Ci5H9F3N2O4: 338; found: 339 [M+H]. 7-nitro-2-(3- (trifluoromethoxy)phenyl)isoindolin-l-one 6 was converted to the corresponding amine and then coupled to various acids as in Steps 3-4 of Example 1 to producevarious compounds of the formula: . See for example, Compound 108.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Trifluoromethoxyaniline, its application will become more common.

Reference:
Patent; SIRTRIS PHARMACEUTICALS, INC.; VU, Chi, B.; MCPHERSON, Lauren; NG, Pui, Yee; BLUM, Charles; WO2010/77686; (2010); A1;,
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Adding a certain compound to certain chemical reactions, such as: 588-96-5, name is p-Bromophenetole, 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 588-96-5, Safety of p-Bromophenetole

To a solution of tert-butyl 4-(piperazinyisulfonyl)perhydro-2H-pyran-4-carboxyate (715 mg, 2.14 mmol, supplied by CarboGen) in toluene (15 mL) under N2 were added 1-bromo-4-ethoxybenzene (473 mg, 2.35 mmol), sodium tert-butoxide (514 mg, 5.35 mmol), palladium(II) acetate (5.0 mg, 0.021 mmol), and tri-tert-butylphosphine (3.5 mg, 0.17 mmol). The reaction was continued overnight at 60 C. under N2. No starting material remained at this time, so the reaction mixture was diluted with methanol and concentrated under reduced pressure. The residue was partially dissolved in dichloromethane and filtered. The filtrate was concentrated under reduced pressure, and the resulting dark material was triturated with diethyl ether to produce a white solid, which was collected by suction filtration to produce 640 mg of clean product (66%). 1H NMR and mass spectrometry (MH+=455) were consistent with the desired structure.

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; Barta, Thomas E.; Becker, Daniel P.; Bedell, Louis J.; Boehm, Terri L.; Brown, David L.; Carroll, Jeffery N.; Chen, Yiyuan; Fobian, Yvette M.; Freskos, John N.; Gasiecki, Alan F.; Grapperhaus, Margaret L.; Heintz, Robert M.; Hockerman, Susan L.; Kassab, Darren J.; Khanna, Ish K.; Kolodziej, Stephen A.; Massa, Mark A.; McDonald, Joseph J.; Mischke, Brent V.; Mischke, Deborah A.; Mullins, Patrick B.; Nagy, Mark A.; Norton, Monica B.; Rico, Joseph G.; Schmidt, Michelle A.; Stehle, Nathan W.; Talley, John J.; Vernier, William F.; Villamil, Clara I.; Wang, Lijuan J.; Wynn, Thomas A.; US2005/9838; (2005); A1;,
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Electric Literature of 64465-53-8, 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. 64465-53-8, name is 4-Fluoro-3-methoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To stirred hydrochloric acid (100 mL) at 0 C. was added 3-methoxy-4-fluoroaniline (10 g, 71 mmol) followed by water (10 mL) and more hydrochloric acid (10 mL). The mixture was warmed to room temperature, stirred for 20 min then cooled to -5 C. A solution of sodium nitrite (5.14 g, 75 mmol) in water (25 mL) was added dropwise such that the internal temperature remained below 0 C. The mixture was warmed to room temperature and stirred for 2 h. The mixture was cooled to -5 C. and a solution of tin(II)chloride dihydrate (64 g, 284 mmol) in hydrochloric acid (200 mL) was added dropwise such that the internal temperature remained below 0 C. The mixture was warmed to room temperature, stirred for 3 h then filtered. The filter cake was washed with hydrochloric acid and dried under vacuum to give a pink solid (7.4 g). The precipitate from the combined filtrates was filtered-off, washed (hydrochloric acid) and dried under vacuum to give a further crop of product (1.8 g. to give a combined yield of 9.2 g, 67%).

The synthetic route of 4-Fluoro-3-methoxyaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Vernalis Research Limited; US6706750; (2004); B1;,
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