Month: July 2021

Related Products of 25245-34-5, The chemical industry reduces the impact on the environment during synthesis 25245-34-5, name is 2-Bromo-1,4-dimethoxybenzene, I believe this compound will play a more active role in future production and life.

Example 7: Preparation of 4,4′-dibromo-2,2′,5,5′- tetramethoxybiphenyl (7); [00113] In a 100 ml round-bottom flask, 3.0 g of FeCI3 in 20 ml of CH2CI2 was added to a solution of 5.0 g of 2,5-dimethoxybromobenzene in 50 ml of CH2CI2. The reaction mixture was stirred overnight, and then it was washed with water and brine and dried with magnesium sulfate. The solvent was removed on a rotary evaporator and the residue was purified by column chromatography eluted by hexane/CH2CI2 (3:1) to obtain 3.4 g of 4,4′- dibromo-2,2′,5,5′-tetramethoxybiphenyl (yield 68%) 1HNMR (CDCI3) 57.194 (s, 2 H), 6.841 (s, 2 H), 3.877 (s 3 H), 3.757 (s, 3 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, 2-Bromo-1,4-dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; AGENCY FOR SCIENCE, TECHNOLOGY AND RESEARCH; NATIONAL UNIVERSITY OF SINGAPORE; WO2006/93467; (2006); A1;,
Ether – Wikipedia,
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Some common heterocyclic compound, 2398-37-0, name is 1-Bromo-3-methoxybenzene, molecular formula is C7H7BrO, 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. category: ethers-buliding-blocks

General procedure: A typical procedure for Suzuki reaction is as follows: arylhalide (0.5mmol) was weighed in 25mL round bottom flask containing boronic acids (0.6mmol), and Pd(OAc)2(PPh3)2/MgCe-HDC (100mg). The reactants and catalyst were dispersed in water (4mL), the RB was mounted on an oil bath at 353K and the mixture was stirred for 2h. The reaction was monitored by thin layer chromatography (TLC). After completion of the reaction, the catalyst was separated by filtration. Then the solution was extracted with ethyl acetate and brine solution. The organic phase was dried over anhydrous Na2SO4 and concentrated under vacuum. The crude product was purified by column chromatography on silicagel to afford pure product. The pure product was analyzed using 1H- and 13C-NMR techniques and compared with literature NMR data.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2398-37-0, its application will become more common.

Reference:
Article; Tomar, Ravi; Singh, Nidhi; Kumar, Neeraj; Tomar, Vartika; Chandra, Ramesh; Catalysis Letters; (2019);,
Ether – Wikipedia,
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Synthetic Route of 5111-65-9, These common heterocyclic compound, 5111-65-9, name is 2-Bromo-6-methoxynaphthalene, 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.

Reference Example 22 Preparation of 2-formyl-6-methoxynaphthalene n-BuLi in hexane (1.59M, 125 ml) was added dropwise to a solution of 2-bromo-6-methoxynaphthalene (42.27 g) in THF (600 ml) at -78 C. and was stirred at -78+ C. for 30 minutes. To the mixture was added DMF (28 ml), and the whole was allowed to warm to room temperature. The reaction mixture was acidified with HCl and extracted with ethyl acetate. The extract was dried and concentrated to give the titled compound (32.31 g) as a colorless solid. 1H-NMR (CDCl3) delta: 3.96 (3H, s), 7.15-7.30 (2H,m), 7.75-7.97(3H,m), 8.26 (1H,s), 10.10 (1H,s). IR (KBr): 2841, 1688, 1624, 1480, 1269, 1028, 856 cm-1.

The synthetic route of 5111-65-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Takeda Chemical Industries, Ltd.; US6420375; (2002); B1;,
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Adding a certain compound to certain chemical reactions, such as: 36865-41-5, name is 1-Bromo-3-methoxypropane, 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 36865-41-5, Application In Synthesis of 1-Bromo-3-methoxypropane

To a solution of ethyl (2E) -3- (2-{ [3-chloro-5- (trifluoromethyl) pyridin-2-yl] oxy}-4-hydroxyphenyl) acrylate (5.10 g) in N, N-dimethylformamide (26 ml); were added potassium carbonate (2.75 g) , sodium iodide (5.90 g) and l-bromo-3- methoxypropane (2.61 g) , and the mixture was stirred at 500C for 1 hr. After allowing to cool to room temperature, IN hydrochloric acid was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried (MgSCM) r filtrated and concentrated. The obtained residue was subjected to silica gel column chromatography, and eluted with ethyl ? acetate-hexane (1:19 – 2:3, v/v) to give a white solid. Recrystallization from ethyl acetate-hexane gave ethyl (2E) -3- [2-{ [3-chloro-5- (trifluoromethyl) pyridin-2-yl] oxy}-4- (3- methoxypropoxy) phenyl] acrylate (4.22 g, yield: 70%) as white ‘ crystals, melting point 86.4-86.5C.

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

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2007/18314; (2007); A2;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Application of 707-07-3, The chemical industry reduces the impact on the environment during synthesis 707-07-3, name is (Trimethoxymethyl)benzene, I believe this compound will play a more active role in future production and life.

General procedure: N -(2-aminobenzoyl)benzotriazoles (0.25 mmol) 1 previously synthesized by our group were reacted with orthoester (0.50 mmol) 2 and ammonium acetate (1.0 mmol) in dioxane for 6-10 h. After completion of the reaction, the solvent was evaporated under reduced pressure. The reaction mixture was purified by column chromatography over silica gel with a EtOAc/n-hexane mixture (from 1:2 or 1:1) to obtain white crystals (62%-95%).

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, (Trimethoxymethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; ?enol, ?lbilge Merve; Celik, ?lhami; Avan, ?lker; Turkish Journal of Chemistry; vol. 43; 6; (2019); p. 1580 – 1596;,
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These common heterocyclic compound, 1535-75-7, name is 2-(Trifluoromethoxy)aniline, 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. COA of Formula: C7H6F3NO

General procedure: Commercially available substituted aniline (63.4mmol) was portionwise added to a solution of concentrated HCl (13mL), ethanol (20mL) and water (7mL). To the above mixture was added dropwise a solution of NaNO2 (4.69g, 69.7mmol) in water (15mL) at 0-5C. After the completion of addition, the reaction mixture was stirred at this temperature for 30min, and then added into a mixture of ethyl 2-chloroacetoacetate (10.88g, 63.4mmol), anhydrous sodium acetate (15.60g, 190.10mmol), and water (90mL) at 0C. The reaction mixture was stirred at 0C for 10min and then at room temperature for 4h. The solid which precipitated was collected by filtration and recrystallized from ethanol to afford light yellow solids (21a-21m) in 75.2-90% yields. 6.3.8 Ethyl 2-chloro-2-(2-(2-(trifluoromethoxy)phenyl)hydrazono)acetate (21h) Light yellow solid; Yield: 90%; M.p.: 93-94 C; MS (ESI) m/z(%): 333.1 [M+Na]+.

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

Reference:
Article; Liu, Ju; Nie, Minhua; Wang, Yanjing; Hu, Jinxing; Zhang, Feng; Gao, Yanlin; Liu, Yajing; Gong, Ping; European Journal of Medicinal Chemistry; vol. 123; (2016); p. 431 – 446;,
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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. 126-38-5, name is 1-Bromo-2,2-dimethoxypropane, A new synthetic method of this compound is introduced below., name: 1-Bromo-2,2-dimethoxypropane

The thioamide from above (0.36 g, 1.63 mmol, 1.0 eq) was suspended in EtOH (10 mL, absolute) under argon at rt. 1-Bromo-2,2-dimethoxypropane (0.22 mL, 1.63 mmol, 1.0 eq) was added via syringe and stirring continued for 72 h at rt. The mixture was then heated to 70 C. for 16 h and concentrated in vacuo. Mass spectrometric analysis of the crude residue was consistent with a corresponding thiazole structure, and no further manipulation was performed before removal of the Boc protecting group in the next step. ESI-MS (m/z) 257 [M+H]+, 201 [M-tBu]+, 157 [M-Boc]+.

The synthetic route of 126-38-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Erickson, Shawn David; Baldwin, John J.; Dolle III, Roland Ellwood; Inglese, James; Ohlmeyer, Michael H.J.; Ho, Koc-Kan; Bohnstedt, Adolph C.; Kultgen, Steven G.; Conti, Paolo Giovanni Martino; Leysen, Dirk; van der Louw, Jaap; US2004/87601; (2004); A1;,
Ether – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 24599-58-4, name is 2,5-Dimethoxytoluene, 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 24599-58-4, Computed Properties of C9H12O2

Preparation of 2,5-dimethoxy-4-methylacetophenone. 1 mol (152 g) of 2,5-dimethoxytoluene is introduced, whilst stirring, into 230 ml of acetyl chloride at -10 C. 160 g of aluminium chloride are then added in the course of 3 hours, whilst stirring and keeping the temperature of the reaction medium at between -10 and 0 C. When the addition has ended, the mixture is stirred for a further 3 hours at between -10 and 0 C. The reaction medium is then poured onto 1 kg of crushed ice to which 110 ml of hydrochloric acid (d=1.19) have been added. After a few hours, the reaction product which has precipitated is filtered off. After washing with water, a 2 N solution of sodium hydroxide and then again with water, the 2,5-dimethoxy-4-methylacetophenone is recrystallized from ethanol. After drying in vacuo, it melts at 75 C.

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; Bugaut; Andree; Grollier; Jean-Francois; Vandenboosche; Jean-Jacques; US4185958; (1980); 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. 54314-84-0, name is ((3-Bromopropoxy)methyl)benzene, A new synthetic method of this compound is introduced below., category: ethers-buliding-blocks

To a mixture of 1-(2-hydroxyethyl)-4-[2-(4-hydroxyphenyl)ethyl]-3-(2,3,4,6-tetra-O-pivaloyl-beta-D-glucopyranosyloxy)-1H-indazole (2 g), cesium carbonate (1.64 g) and sodium iodide (0.38g) in N,N-dimethylformamide (10 mL) was added benzyl 3-bromopropyl ether (0.86 g), and the mixture was stirred at room temperature overnight. The reaction mixture was poured into water, and the resulting mixture was extracted with diethyl ether. The extract was washed with water and brine, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was dissolved in dichloromethane (15 mL). To the solution were added triethylamine (1.22 mL) and pivaloyl chloride (0.93 mL), and the mixture was stirred at room temperature overnight. The reaction mixture was poured into 0.5 mol/L hydrochloric acid, and the resulting mixture was extracted with diethyl ether. The extract was washed with water, a saturated aqueous sodium hydrogen carbonate solution and brine, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate = 3/1) to give 4-{2-[4-(3-benzyloxypropoxy)phenyl]ethyl}-3-(2,3,4,6-tetra-O-pivaloyl-beta-D-glucopyranosyloxy)-1-(2-pivaloyloxyethyl)-1H-indazole (2.11 g). This material was dissolved in ethyl acetate (20 mL). To the solution was added 10percent palladium-carbon powder (0.5 g), and the mixture was stirred at room temperature under a hydrogen atmosphere for 2 hours. The insoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate = 2/1 – 1/1) to give the title compound (1.59 g). 1H-NMR (CDCl3) delta ppm: 1.02 (9H, s), 1.03 (9H, s), 1.13 (9H, s), 1.15 (9H, s), 1.17 (9H, s), 2.0-2.1 (2H, m), 2.8-2.9 (1H, m), 2.9-3.0 (1H, m), 3.0-3.15 (1H, m), 3.2-3.3 (1H, m), 3.8-3.9 (2H, m), 3.9-4.0 (1H, m), 4.05-4.2 (3H, m), 4.21 (1H, dd, J=12.4Hz, 1.6Hz), 4. 3-4. 5 (4H, m), 5.2-5.3 (1H, m), 5.35-5.55 (2H, m), 6.05 (1H, d, J=7.8Hz), 6.64 (1H, d, J=6.9Hz), 6.75-6.85 (2H, m), 7.0-7.1 (3H, m), 7.15-7.2 (1H, m)

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; Kissei Pharmaceutical Co., Ltd.; EP1724278; (2006); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 175278-17-8,Some common heterocyclic compound, 175278-17-8, name is 2-Bromo-4-(trifluoromethoxy)aniline, molecular formula is C7H5BrF3NO, 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.

A mixture of 2-bromo-4-(trifluoromethoxy)aniline 17 (Maybridge, 2.048 g, 8.00 mmol), methyl acrylate (1.80 mL, 20.0 mmol), Pd(OAc)2 (215.5 mg, 0.960 mmol), tri-o-tolylphosphine (1.169 g, 3.84 mmol), and dry Et3N (4.30 mL, 30.9 mmol) in dry CH3CN (16.0 mL) was stirred under reflux conditions under N2 for 4 h, then concentrated in vacuo. The residue was partitioned between H2O (30 mL) and AcOEt (30 mL). The organic layer was separated and the aqueous layer was extracted with AcOEt (30 mL × 2). The organic layers were combined, dried over anhydrous MgSO4, filtered, and concentrated in vacuo to afford 3.630 g of the title product 21 (crude). This compound was used for the next step without further purification. 1H NMR (270 MHz, CDCl3) delta 7.74 (1H, d, J = 15.8 Hz), 7.23-7.02 (2H, m), 6.68 (1H, d, J = 8.72 Hz), 6.36 (1H, d, J = 15.8 Hz), 4.00 (2H, br s), 3.81 (3H, s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-4-(trifluoromethoxy)aniline, its application will become more common.

Reference:
Article; Hayashi, Shigeo; Ueno, Naomi; Murase, Akio; Nakagawa, Yoko; Takada, Junji; European Journal of Medicinal Chemistry; vol. 50; (2012); p. 179 – 195;,
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