Month: May 2021

Synthetic Route of 38603-09-7, A common heterocyclic compound, 38603-09-7, name is 1,3-dibromo-2-methoxybenzene, molecular formula is C7H6Br2O, 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.

Example 21 Preparation of (3-Bromo-2-methoxyphenyl)-(2-methoxyphenyl)methanol 2,6-Dibromoanisole (138.0 g, 0.51 mol) was dissolved in 750 ml of tetrahydrofuran and the solution cooled to -63 C. Butyl lithium (319 ml of 1.6 M, 0.51 mol) was added slowly with stirring and the mixture stirred at -60 C. for 4.5 hours and then 69.4 g (0.51 mol) of o-anisaldehyde in 250 ml of tetrahydrofuran was added slowly with stirring and the mixture allowed to stir cold for 1 hour. The mixture was allowed to warm to ambient temperature and was then poured into a mixture of ice and saturated aqueous ammonium chloride. The resulting mixture was extracted with ether and the ether extract dried over magnesium sulfate and then concentrated by evaporation under reduced pressure to obtain the title compound. This was purified by preparative liquid chromatography eluding with a 5:95 mixture of ethyl acetate and hexane to obtain 44.6 g (24 percent of theory) of material having a proton nmr spectrum consistent with the assigned structure.

The synthetic route of 38603-09-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The Dow Chemical Company; US4979978; (1990); A;,
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Reference of 2186-92-7, A common heterocyclic compound, 2186-92-7, name is P-anisaldehyde dimethyl acetal, molecular formula is C10H14O3, 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.

General procedure: Under an atmosphere of argon, to a mixture of benzaldehyde (0.213 g, 2.0 mmol) and Al-MCM-41 (60 mg, dried prior to use at 120C for 1 h under vacuum) in acetonitrile (3.0 mL), 1-phenyl-1-trimethylsiloxyethene (0.462 g, 2.4 mmol) in acetonitrile (3.0 mL) was added through a syringe at 0C. The reaction mixture wasstirred at 0C for 15 min. The catalyst was removed by filtration and washed with Et2O (40 mL). After the filtrate was concentrated under reduced pressure, crude product was purified by silica-gel column chromatography (hexane/Et2O 20:1) to give 1,3-diphenyl-3-trimethylsiloxypropan-1-one as a colorless oil (0.591 g, 99%). The recovered catalyst was dried at 70C for 15 min. The catalyst (47 mg) was then dried at 120C for 1 h under vacuum and used in a second run.

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:
Article; Ito, Suguru; Tanuma, Kenji; Matsuda, Kohei; Hayashi, Akira; Komai, Hirotomo; Kubota, Yoshihiro; Asami, Masatoshi; Tetrahedron; vol. 70; 45; (2014); p. 8498 – 8504;,
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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. 4457-67-4, name is 1-Bromo-4-methoxybutane, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-4-methoxybutane

A solution of 4-methoxybutyl bromide (4.5 g) in acetonitrile (15 ml) is added dropwise under reflux to a mixture of salicylic acid ethyl ester (2.63 ml), powdered potassium carbonate (3.10 [G)] and potassium iodide (10 mg) in acetonitrile (50 ml), and the reaction mixture is then stirred overnight. After cooling, filtration is carried out, the filtrate is concentrated and the residue is added under a high vacuum. The title compound (4.4 g), Rf (C) =0.28, is obtained in the form of a pale-yellow oil.

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; ELAN PHARMACEUTICALS, INC.; WO2003/103652; (2003); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 1000574-79-7, name is 2-Bromo-4-(difluoromethoxy)aniline, 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 1000574-79-7, Recommanded Product: 1000574-79-7

Into a 250-mL round-bottom flask purged with and maintained under nitrogen was placed 2- bromo-4-(difluoromethoxy)benzenamine (7.9 g, 33.2 mmol), dioxane (100 mL), water (10 mL), CS2CO3 (32.46 g, 99.63 mmol), 4,4,5,5-tetramethyl-2-(prop-l-en-2-yl)-l,3,2-dioxaborolane (8.36 g, 49.8 mmol), and Pd(dppf)Cl2 (1.21 g, 1.65 mmol). The resulting solution was stirred overnight at 90C. The solids were filtered out. The filtrate was concentrated under vacuum. The residue was applied onto a silica gel column and eluted with a gradient of ethyl acetate/petroleum ether (1 :30 to 1 :20). This resulted in 5.3 g (80%) of the title compound as a yellow solid. MS-ESI: 200.1 (M+l).

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-Bromo-4-(difluoromethoxy)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; IFM TRE, INC.; GLICK, Gary; ROUSH, William R.; VENKATRAMAN, Shankar; SHEN, Dong-Ming; GHOSH, Shomir; KATZ, Jason; SEIDEL, Hans Martin; FRANCHI, Luigi; WINKLER, David Guenther; OPIPARI JR., Anthony William; (783 pag.)WO2019/23147; (2019); A1;,
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92028-21-2, name is 6-Methoxy-[1,1′-biphenyl]-3-amine hydrochloride, 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. COA of Formula: C13H14ClNO

d. Synthesis of N-{2-[4-(3-phenyl-4-methoxyphenyl)aminophenyl]ethyl}-(R)-2-tert-butyldimethylsilyl-2-(8-benzyloxy-2(1H)-quinolinon-5-yl)ethylamine (NN); To compound JJ hydrochloride (73.7 g, 114 mmol) and 4-methoxy-3-phenylaniline hydrochloride (32.4 g, 137 mmol), toluene (380 mL) was added with mild agitation for 5 minutes, followed by sodium tert-butoxide (49.3 g, 513 mmol) in portions over 1 minute, and finally 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (10.65 g, 17 mmol) and tris(dibenzylideneacetone)dipalladium(0) (5.22 g, 5.7 mmol). The resulting mixture was stirred and heated to 85-89 C. (internal) for 2.5 hours. The solution was cooled to room temperature, water (400 ml) was added and the mixture was stirred for 5 minutes, filtered through Celite (80 g), and partitioned with toluene (100 ml). The organic layer was collected and concentrated under reduced pressure in a 40 C. bath to give N-{2-[4-(3-phenyl-4-methoxyphenyl)aminophenyl]ethyl}-(R)-2-tert-butyldimethylsilyl-2-(8-benzyloxy-2(1H)-quinolinon-5-yl)ethylamine (NN) as a dark viscous oil.

The synthetic route of 92028-21-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Axt, Sabine; Stergiades, Ioanna; US2004/224982; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 1313876-00-4, 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. 1313876-00-4, name is 4,7-Dibromo-5,6-bis(dodecyloxy)benzo[c][1,2,5]thiadiazole belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

4,7-dibromo-5,6-bis (dodecyloxy) benzo [c] [1,2,5] thiadiazole(2.65 g, 4 mmol),Compound A-1 (5.53 g, 10 mmol),Pd (PPh3) 4 (0.23 g, 0.2 mmol),25 mL of dimethylformamide (DMF) was added to toluene (75 mL), and the mixture was heated at 90, 100, and 110 C for 48 hours.After cooling the reaction, the residue was precipitated in methanol and filtered. The separated organic layer was washed with water. Thereafter, the mixture was subjected to vacuum distillation and purified by flash chromatography with methylene chloride and chloroform. The solid was washed with a large amount of methanol and dried under vacuum for 24 hours. To obtain a dark violet powder compound 1-1 (4.3 g, 84%).

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, 4,7-Dibromo-5,6-bis(dodecyloxy)benzo[c][1,2,5]thiadiazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; LG Chem, Ltd.; Im Bo-gyu; Lee Jae-cheol; Lee Haeng-geun; Park Jeong-hyeon; (24 pag.)KR2017/126689; (2017); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 2338-54-7, 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. 2338-54-7, name is 4-Fluoro-3-methylanisole, This compound has unique chemical properties. The synthetic route is as follows.

To a 250 mL three-necked flask was added 1-fluoro-4-methoxy-2-methylbenzene (18.3 g, 130.6 mmol)Under ice-cooling, sulfonyl chloride (27.4 g, 235.0 mmol) was slowly added dropwise and reacted at room temperature for 2 h. After completion of the reaction, the reaction solution was poured into ice water and analyzed.A large amount of solid was added, and the filter cake was dried in vacuo to give 23.2 g of 5-fluoro-2-methoxy-4-toluenesulfonyl chloride in 74.5% yield.

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

Reference:
Patent; Guizhou University; Liu Li; Quan Wen; Zhang Menghui; Huang Zhuyan; (6 pag.)CN106674065; (2017); A;,
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. 13985-15-4, name is 2,3,6,7-Tetramethoxy-9,10-dimethylanthracene, A new synthetic method of this compound is introduced below., Safety of 2,3,6,7-Tetramethoxy-9,10-dimethylanthracene

The result of step 2A-1, 2,3,6,7-tetrakis (methoxy) -9,10-dimethyl anthracene(10.0 g), sodium dichromate (50 g),Acetic acid (500 ml) was refluxed for 60 minutes to obtain 2,3,6,7-tetrakis (methoxy) anthracene-9,10-dione (2)

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; Hanyang University Industry-Academic Cooperation Foundation; Seo Dong-hak; Choi Gyeong-hwan; (85 pag.)KR2018/43221; (2018); 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. 4457-67-4, name is 1-Bromo-4-methoxybutane, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1-Bromo-4-methoxybutane

d) Benzyl (3R,4R,5S)-3-hvdroxy-4-[4-(4-methoxy-butoxy)phenvH-5-thiso- propylsilanyloxy-piperidine-1-carboxylate; Analogously to method F, starting from benzyl (3R,4R,5S)-3-hydroxy-4-[4- hydroxyphenyl]-5-triiso-propylsilanyloxypiperidine-1 -carboxylate [873945-27-8] and 1 -bromo-4-methoxybutane [4457-67-4] the title compound is obtained as a yellow oil. Rt = 6.63 (gradient I).; General method F: (phenol alkylation I); The mixture of 20 mmol of “phenol” in 60 ml of N,N-dimethylformamide is stirred with 4.15 g of potassium carbonate and 30 mmol of “halide” or “tosylate” for 24 hours at 1000C. The reaction mixture is then evaporated. The residue is treated with 1 M aqueous sodium hydrogencarbonate solution (40 ml) and extracted with ethyl acetate (2 X 60 ml). The organic phases are washed with brine (1 X 60 ml), dried using sodium sulphate and evaporated. The title compound is obtained from the residue by means of flash chromatography (SiO2 60F).

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 4457-67-4.

Reference:
Patent; Speedel Experimenta AG; WO2008/17685; (2008); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

These common heterocyclic compound, 104566-41-8, name is (3-(Benzyloxy)phenyl)methanamine hydrochloride, 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. name: (3-(Benzyloxy)phenyl)methanamine hydrochloride

N(3-benzyloxy-benzyl)-4-biphenylacetamide; To a solution of 4-biphenyl acetic acid (2.29 g, 10.45 mmol) in dimethylformamide, DMF, (30 ml) was added diisopropylethylamine, DIEA, (5.47 ml, 31.35 mmol) and stirred at room temperature for 15 min, then benzotriazolyloxy-tris[pyrrolidino]-phosphonium hexafluorophosphate, PyBOP, (5.43 g, 10.45 mmol) was added and the stirring was continued for further 30 min, then 3-benzyloxybenzylaminehydrochloride (2.6 g, 10.45 mmol) was added and the stirring continued for 24 hrs. The reaction mixture was then poured on to ice cooled water acidified with (10 ml) 1 N HCl and extracted with ethyl acetate (100 ml) and the organic layer washed with saturated solution of NaHCO3, water and brine, dried over Na2SO4 and the solvent removed under vacuum to give a yellowish-white powder of the desired compound (2.65 g) 62% yield.

The synthetic route of (3-(Benzyloxy)phenyl)methanamine hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hangauer, David G.; US2006/160800; (2006); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem