Author: Jessica.F

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. 39538-68-6, name is 2-Methoxy-4-methylaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 2-Methoxy-4-methylaniline

General procedure: To a magnetically-stirred, ice-bathed, solution of substituted aniline (1 equiv) in acetone (20 mL) at 0 C was added cyanuric chloride (1 equiv), and the resulting mixture was stirred at 0 C for 2 h and then at room temperature for an additional 2 h. Subsequently, crushed ice (10 mL) was added to the reaction, and the mixture was allowed to warm up to room temperature over 1 h. The solid was collected by vacuum filtration and was washed with water three times (3-10 mL).45

The synthetic route of 39538-68-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Shahin, Rand; Taha, Mutasem O.; Bioorganic and Medicinal Chemistry; vol. 20; 1; (2012); p. 377 – 400;,
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Electric Literature of 458-03-7, The chemical industry reduces the impact on the environment during synthesis 458-03-7, name is 1-Ethoxy-3-fluorobenzene, I believe this compound will play a more active role in future production and life.

EXAMPLE 92 To 29.8 g of 2,3-dichloro-4-methoxybenzoyl chloride in 150 ml of 1,2-dichloroethane, 16.3 g of m-fluorophenetole is added. The solution is chilled to 5 C. as 16.5 g of aluminum chloride is added slowly. After 2 hr, the reaction mixture is worked up with water and diethyl ether to give a mixture of 2,3-dichloro-4′-ethoxy-2′-fluoro-4-methoxybenzophenone and 2,3-dichloro-2′-ethoxy-4′-fluoro-4-methoxybenzophenone. The mixture is separated by preparative high pressure liquid chromatography (10% ethyl acetate/hexane 250 ml/min) to give 2,3-dichloro-4′-ethoxy-2′-fluoro-4-methoxybenzophenone, mp 94-96 C. Analysis: Calculated for C16 H13 Cl2 FO3: 55.99%C; 3.82%H. Found: 55.86%C; 3.81%H.

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-Ethoxy-3-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hoechst-Roussel Pharmaceuticals, Inc.; US4673746; (1987); 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. 53087-13-1, name is 1-(Benzyloxy)-3-bromobenzene, A new synthetic method of this compound is introduced below., Product Details of 53087-13-1

A 1 L round-bottomed flask was charged with 1-(benzyloxy)-3-bromobenzene (45.5 g, 173 mmol), tert-amyl alcohol (200 mL) and dioxane (400 mL), and the contents were sparged with N2 for 45 minutes. A 3 L round-bottomed flask was charged with potassium phosphate tribasic (92 g, 433 mmol), 1,3-cyclohexanedione (97 weight %, 20 g, 173 mmol), palladium(II) acetate (0.78 g, 3.5 mmol) and 2-(di-tert-butylphospino)-2?-methylbiphenyl (2.16 g, 6.9 mmol), and the contents were sparged with N2 for 45 minutes. The solution of 1-(benzyloxy)-3-bromobenzene was then transferred to the 1,3-cyclohexanedione mixture via cannula, and the reaction mixture was heated to reflux overnight. The reaction mixture was cooled to room temperature and partitioned between ethyl acetate (600 mL) and 10% hydrochloric acid (600 mL) with mixing. The lower aqueous layer was separated and extracted with ethyl acetate (600 mL). The combined organic layers were washed with brine (2×100 mL) and concentrated under reduced pressure. The residue was taken up in toluene (300 mL) and again concentrated under reduced pressure. The residue was taken up in toluene (300 mL) and warmed to 50 C. After cooling to room temperature, the solids were collected by filtration, washed with toluene (2×50 mL) and dried in a vacuum oven at 50 C. to give the titled compound (44.6 g, 88%). 1H NMR (400 MHz, DMSO-d6) delta ppm 10.54 (bs, 1H), 7.46-7.28 (m, 5H), 7.19-7.13 (m, 1H), 6.84-6.79 (m, 1H), 6.75-6.72 (m, 1H), 6.71-6.66 (m, 1H), 5.03 (s, 2H), 2.76-2.13 (m, 4H), 1.99-1.86 (m, 2H); MS (CI-NH3) m/z 312.0 (M+NH4)+.

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; AbbVie Inc.; Reata Pharmaceuticals, Inc.; Donner, Pamela; Wagner, Rolf; Shanley, Jason; Heyman, Howard; Krueger, Allan; Chen, Hui-Ju; Rozema, Michael; Grampovnik, David; Visnick, Melean; Anderson, Eric; Jiang, Xin; Bender, Christopher F.; Bolton, Gary Louis; Caprathe, Bradley William; Lee, Chitase; Roark, William Howard; US2015/225397; (2015); A1;,
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Synthetic Route of 89282-70-2, 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. 89282-70-2, name is 2-Methoxy-2-methylpropan-1-amine, This compound has unique chemical properties. The synthetic route is as follows.

In a round bottom flask under nitrogen 100 mg (0.23 mmol) of intermediate Awas dissolved in 4 mL ofCH2Ch and 0.12g ofDIPEA (0.92 mmol) was added followed by 108mg (0.7 mmol) of 2-Methoxy-2-methyl-propylamine. The mixture was allowed to stir overnight and then condensed in vacuo. The residue was dissolved in 20 mL ofEtOAc andwashed with 2x 20 mL of water, 20 mL of brine, dried over Na2S04 and condensed in vacuo.Purification by biotage flash chromatography (Si02, MeOH/CH2Ch/Et3N gradient) affords 71mg of the title compound as a clear viscous oil

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

Reference:
Patent; ZAFGEN, INC.; ZAHLER, Robert; VATH, James, F.; WO2013/169860; (2013); 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. 53087-13-1, name is 1-(Benzyloxy)-3-bromobenzene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 1-(Benzyloxy)-3-bromobenzene

The 2-(3-hydroxyphenyl)-2,3-dimethoxypropan-1-ol, used as a starting material, was obtained as follows: Methoxyaceonitrile (14 g) in tetrahydrofuran (10 ml) was added to a solution of 3-benzyloxyphenylmagnesium bromide [prepared by heating a mixture of 3-benzyloxybromobenzene (52.6 g), magnesium powder (4.8 g) and tetrahydrofuran (250 ml) to 60 C. for 3 hours] in tetrahydrofuran and the mixture was heated to 60 C. for 30 minutes. The mixture was cooled to ambient temperature and acidified by the addition of 3N hydrochloric acid solution (250 ml). The mixture was extracted with diethyl ether. The organic phase was washed with water and with a saturated aqueous sodium chloride solution, dried (MgSO4) and evaporated. The residue was purified by column chromatography using a 19:1 v/v mixture of methylene chloride and diethyl ether as eluent. There was thus obtained 3-benzyloxyphenyl methoxymethyl ketone (32.3 g, 63%), as an orange oil.

The synthetic route of 53087-13-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Imperial Chemical Industries PLC; ICI Pharma; US5132328; (1992); A;,
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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 74137-36-3 as follows. Application In Synthesis of 1,3-Dibromo-5-methoxybenzene

[3-(3-Bromo-5-cyano-phenoxy)-4-chloro-2-fluoro-phenyl]-acetic Acid Ethyl Ester (R-20c) step 1-n-BuLi (2.6 mL of a 1.6 M solution, 1.1 equiv) was added slowly to a solution of the R-21a (1.0 g, 3.8 mmol, CAS Reg. No. 74137-36-3) in Et2O (20 mL) cooled to -78 C. under an N2 atmosphere. The solution was stirred for 45 min, and DMF was added via syringe. The solution was warmed slowly to RT, added to saturated ammonium chloride, and extracted with ether. The organic phase was washed with brine and dried (MgSO4), filtered and evaporated to afford 0.80 g (98%) of R-21b.

According to the analysis of related databases, 74137-36-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Billedeau, Roland Joseph; Sweeney, Zachary Kevin; US2009/170856; (2009); 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. 5467-58-3, name is 1-Bromo-4-methoxynaphthalene belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: ethers-buliding-blocks

3-a. Synthesis of 1-methoxy-4-{4-(naphthalen-1-yl)phenyl}naphthalene 1-Methoxy-4-{4-(naphthalen-1-yl)phenyl} was synthesized as follows. 1-Bromo-4-methoxynaphthalene (25 g, 0.105 mol), 4-(naphthalen-1-yl)phenylboronic acid (30.4 g, 0.137 mol), potassium carbonate (21.9 g, 0.16 mol), tetrakis(triphenylphosphine)palladium(0) (2.4 g, 0.01 mol), water (25 mL), tetrahydrofuran (75 mL) and toluene (75 mL) were stirred in a 250 mL round-bottom flask for 12 hours under reflux. After completion of the reaction, the reaction mixture was cooled to room temperature and extracted with ethyl acetate (300 mL) and water (1000 mL). The organic layer was dried with magnesium sulfate and concentrated under reduced pressure to obtain a solid. The solid was dissolved in hot toluene (400 mL) and then filtered. The filtrate was recrystallized in methanol (800 mL). The resultant solid was filtered and washed with hexane (300 mL) to obtain a product (20 g, 0.055 mol, 52.6%).

The synthetic route of 5467-58-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC CO., LTD.; US2011/108827; (2011); A1;,
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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 20469-65-2 as follows. Safety of 1-Bromo-3,5-dimethoxybenzene

To a solution of 1 (25.0 g, 115.18 mmol) in DCM (200 mL) was added dropwise BBn (21.45 mL, 230.35 mmol) at 0 C, and the mixture was stirred at 25 C for 16 h. The reaction was quenched by MeOH (50 mL) and concentrated under vacuum to afford 2 (21.7 g, 99.7%) as a red oil, which was used directly without further purification.

According to the analysis of related databases, 20469-65-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GENENTECH, INC.; F. HOFFMANN-LA ROCHE AG; DRAGOVICH, Peter; PILLOW, Thomas; BLAKE, Robert Anthony; WERTZ, Ingrid; (619 pag.)WO2020/86858; (2020); A1;,
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Adding a certain compound to certain chemical reactions, such as: 156573-09-0, name is 1-Bromo-4-ethoxy-2,3-difluorobenzene, 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 156573-09-0, category: ethers-buliding-blocks

Under a nitrogen atmosphere,60 g of trimethylsilylacetylene,120 g of 4-ethoxy-2,3-difluorobromobenzene, 1.9 g of copper iodide,11.7 g of tetrakistriphenylphosphine palladium were dissolved in 500 mL of DMF,And the mixture was stirred at 70 C. for 2 hours.To the reaction mixture were added toluene,Add water,After stirring, the organic layer was separated.The organic layer was washed with waterwater,Ammonia water,Followed by washing with saturated saline in this order,After drying with anhydrous sodium sulfate,The solvent was distilled off under reduced pressure.The obtained crystalRecrystallization and purification by column chromatography (silica gel)120 g of trimethyl- (4-ethoxy-2,3-difluorophenylethynyl) silane was obtained.

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; DIC CORPORATION; NOSE, SAYAKA; SAITOU, YOSHITAKA; KADOMOTO, YUTAKA; (18 pag.)JP5696874; (2015); B2;,
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Electric Literature of 17715-69-4, 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. 17715-69-4, name is 1-Bromo-2,4-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A suspension of Pd2(dba)3 (6.9 mg, 0.0075 mmol), tBu3PHBF4 (8.7 mg,0.03 mmol), KOH (42 mg, 0.75 mmol), aryl bromide 9 (0.36 mmol) and tetralone 10(0.3 mmol) in a mixture of dioxane/water (4:1, v/v, 3 mL) was degassed and heated under Ar and microwave irradiation (80W of initial power, 100 °C, 40min, infrared probe). Then, the mixture was allowed to cool to rt, diluted in AcOEt, washed with saturated NH4Cl solution, dried over anhydrous Na2SO4,filtered and concentrated under reduced pressure. The crude material was purified by silica gel chromatography.

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

Reference:
Article; Manvar, Dinesh; Fernandes, Talita De A.; Domingos, Jorge L.O.; Baljinnyam, Erdenechimeg; Basu, Amartya; Junior, Eurides F.T.; Costa, Paulo R.R.; Kaushik-Basu, Neerja; European Journal of Medicinal Chemistry; vol. 93; (2015); p. 51 – 54;,
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