Month: March 2021

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. 171290-52-1, name is 3,5-Dimethoxyphenylacetylene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C10H10O2

General procedure: The azido-sugar 2(1 equiv) was dissolved in dry THF (45 mL/mmol) and the required alkyne derivative (5.4 equiv), diisopropylethylamine(1.9 equiv), CuI (0.57 equiv) and DMEDA (5.2 equiv) were added. The reaction mixture was heated to reflux until TLC indicated complete consumption of 2, then the solvent was removed.The residue was dissolved in EtOAc and washed with H2O twice and once with an aqueous solution of EDTA (1%,m/v). The organic layer was dried over MgSO4, filtered and the solvent removed. Purification of the crude material on column chromatography on silica gel (CH2Cl2/EtOAc) afforded the desired product

According to the analysis of related databases, 171290-52-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Van Nguyen, Tai; Hospital, Audrey; Lionne, Corinne; Jordheim, Lars P.; Dumontet, Charles; Perigaud, Christian; Chaloin, Laurent; Peyrottes, Suzanne; Beilstein Journal of Organic Chemistry; vol. 12; (2016); p. 1476 – 1486;,
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Electric Literature of 2339-58-4, 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. 2339-58-4, name is 3-Fluoro-5-methoxyaniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of 3-(trifluoromethyl)aniline(5.0 g, 31 mmol) and trimethyl orthoformate (4.9 g, 46.5mmol) was added three drops of sulfuric acid.This mixture was slowly heated to 120 oC to allow MeOH to be distilled off, stirred for 2 h at 120 oC, heated to 170 oCfor 30 min, and cooled to 100 oC.Then aq. HCl (10%; 25 mL) was added.This mixture was then refluxed for 3 h, cooled to 0 oC (ice bath) and finally basified with aq. NaOH (20%).This solution was extracted with EtOAc (3 ¡Á 30 mL), dried (MgSO4), filtered, and concentrated under reduced pressure. The crudeproduct was purified on a silica gel column with gradient elution (hexanes hexane-EtOAc; 1: 10 v/v) to afford S7 as a colorless oil

The synthetic route of 3-Fluoro-5-methoxyaniline has been constantly updated, and we look forward to future research findings.

Reference:
Article; Naumiec, Gregory R.; Cai, Lisheng; Pike, Victor W.; Bioorganic and Medicinal Chemistry Letters; vol. 25; 2; (2015); p. 225 – 228;,
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Reference 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 62: 3-(5-Oxo-4,5,6,7,8,9-hexahydro-2H-1,2,7,9-tetraazabenz[f]inden-4-yl)-N-(4-trifluoromethoxy-phenyl)-benzamide; compound with trifluoro-acetic acid Preparation of the aldehyde: to a solution of 300 mg of 4-carboxybenzaldehyde (2 mmoles) and 382 mg of 4-(trifluoromethoxy)aniline (2 mmoles) in 5 ml of ethyl acetate is added 830 mg of dicyclohexycarbodiimide) (DCC) (4 mmoles). The reaction mixture is heated at 60¡ãC overnight and then poured into 60 ml of 1 N HCl solution. The mixture is extracted with twice 30 ml of ethyl acetate. The combined organic phases are washed with 50 ml of water; 50 ml saturated solution of sodium bicarbonate and brine, dried over MgSO4 and evaporated. The crude is purified on silica gel giving 233 mg of 4-Formyl-N-(3-trifluoromethoxy-phenyl)-benzamide (yield=38percent). ([M+H]+): 310). Ret. Time: 5.60 min (gradient 5 to 85 percent acetonitrile in 7 min).

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; Aventis Pharma S.A.; EP1746097; (2007); A1;,
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Reference of 5414-19-7, The chemical industry reduces the impact on the environment during synthesis 5414-19-7, name is 1-Bromo-2-(2-bromoethoxy)ethane, I believe this compound will play a more active role in future production and life.

To a room temperature mixture of the tert-butyl [2- [ (4-BROMOPHENYL) SULFONYL]] acetate (2) from Part A (0.25 mol) in 100 mL dimethyl formamide (“DMF”) was added 18-crown-6 (19.4 g, 0.07 mol), potassium carbonate [(“K2CO3”)] (169 g, 1.22 mol), and bis (2- bromoethyl) ether (62.5 g, 0.27 mol). The mixture was stirred at room temperature for 18 hr, after which time no starting material (2) was detected by HPLC. The resulting mixture was concentrated, diluted in 500 mL ethylacetate [(“CH3COOC2HS”OR”ETOAC”),] and filtered. The resulting filtrate was concentrated to produce a yellow oil that solidified upon standing to afford the desire product (3). LCMS: [M+Na] = 427.05.

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-(2-bromoethoxy)ethane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PHARMACIA CORPORATION; WO2004/811; (2003); A1;,
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Some common heterocyclic compound, 36805-97-7, name is 1,1-Di-tert-butoxy-N,N-dimethylmethanamine, molecular formula is C11H25NO2, 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. Computed Properties of C11H25NO2

C. 3-[5-(3,4-Dichloro-phenyl)-1-(2,4-dichloro-phenyl)-1H-pyrazol-3-yl]-propionic acid tert-butyl ester. To a 3-neck round bottom flask fitted with an air condenser was added 3-[5-(3,4-dichloro-phenyl)-1-(2,4-dichloro-phenyl)-1H-pyrazol-3-yl]-propionic acid (1.0 g, 2.3 mmol, 1.0 equiv) and toluene (23 mL) under nitrogen. The mixture was heated to 80 C. then N,N-dimethyl-di-tert-butylacetal (2.36 g, 11.6 mmol, 5.0 equiv) was added dropwise (neat). The reaction mixture was heated at 80 C. for 1 h then additional N,N-dimethyl-di-tert-butylacetal (2.36 g, 11.6 mmol, 5.0 equiv) was added. This mixture was stirred at 80 C. for 2 h then cooled to room temperature and partitioned between water (100 mL) and ether (100 mL). The organic layer was washed with 1 M sodium hydroxide (50 mL), water (50 mL) then brine (50 mL), dried (Na2SO4), and concentrated under reduced pressure. The crude material was then purified by flash chromatography (20% ethyl acetate/hexanes) to afford the desired ester (1.1 g, >99%). HPLC: Rt=3.59 (Method A). MS (ESI): mass calculated for C22H20Cl4N2O2, 484.03; m/z found, 485.0 [M+H]+. 1H NMR (500 MHz, DMSO-d6): 7.81 (d, J=2.2 Hz, 1H), 7.65 (d, J=8.5 Hz, 1H), 7.61-7.59 (m, 2H), 7.48 (d, J=2.2 Hz, 1H), 7.05 (dd, J=8.2, 1.9 Hz, 1H), 6.71 (s, 1H), 2.87 (t, J=7.4 Hz, 2H), 2.61 (t, J=7.4 Hz, 2H), 1.38 (s, 9H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 36805-97-7, its application will become more common.

Reference:
Patent; Deng, Xiaohu; Mani, Neelakandha; Mapes, Christopher M.; US2006/4195; (2006); A1;,
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Adding a certain compound to certain chemical reactions, such as: 24332-20-5, name is 1,1,2-Trimethoxyethane, 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 24332-20-5, COA of Formula: C5H12O3

Reaction of cis – cedimnylene glycol with methoxyacetaldehyde dimethylacetal24 g (0.1 mol) of cis-cedrylene glycol (using 26 g of a GC content of 92%), 127.6 g (1.45 mol)Methoxyacetaldehyde dimethyl acetal and 0.4 g of concentrated sulfuric acid were stirred at 10 C for 24 hours. At the end of the reaction, methyl tert-butyl was addedEther, washed with a 5% solution of sodium hydrogencarbonate, and the low boiling components removed by distillation. After the addition of n-hexane, unreacted cis-isomer was addedType – cypressane diol crystallization, filtration separation. After concentration of the filtrate by evaporation, 30.4 g of crude product was obtained. According toThe content of the compounds of formulas (X) and (XI) in the product obtained by GC analysis was 51% (corresponding to a theoretical yield of 50%). The originalThe material was dissolved in dipropylene glycol (DPG) to prepare a solution of the compound of formulas (X) and (XI) in an amount of 10% by weightExample (VIII): (IX) = 1: 6.2).For analytical purposes, cyclohexane / ethyl acetate eluant (60/1) was passed through silica gel 60 (0.04-0.063 mm)(X) and (XI) in the crude product were separated from each other by liquid chromatography on a liquid chromatograph. (X)Of the compound has a purity of 99.4% and the purity of the compound of formula (XI) is 96.9%.Compounds of formula (X): & lt; EMI ID =

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, 1,1,2-Trimethoxyethane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Simrose Corporation; Bei, Ende hhuoersiche; (41 pag.)CN105228993; (2016); A;,
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Related Products of 7252-83-7, 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 7252-83-7 as follows.

4-Hydroxythiobenzamide (0.20 mol) and 2-bromo-1,1-dimethoxyethane (0.20 mol) were stirred in ethanol (600 mL) at room temperature and p-toluenesulfonic acid (0.20 mol) was added. Into the reaction solution. Heat to 90 C for 24 h. After the reaction was completed, it was cooled to room temperature, and the solvent was evaporated under reduced pressure, and water (200 mL) was added.The pH was adjusted to 8 with saturated sodium bicarbonate solution, extracted with dichloromethane (200 mL¡Á3), and the organic phases were combined.Concentration under reduced pressure and distillation gave 2-(4-hydroxyphenyl)thiazole.

According to the analysis of related databases, 7252-83-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Ocean University of China; Shao Changlun; (69 pag.)CN108658937; (2018); 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. 3586-14-9, name is 1-Methyl-3-phenoxybenzene, A new synthetic method of this compound is introduced below., COA of Formula: C13H12O

EXAMPLE 1 Into a 200 ml four necked flask equipped with a distillation column, 36.9 g (0.2 mole) of m-phenoxytoluene and 1.0 g of powdery activated carbon were charged and heated at 180 C. while stirring and then, 71.1 g of 1,2-dibromotrichloroethane (0.24 mole) was added dropwise for 30 minutes and the reaction was continued at the temperature for 3 hours. After the reaction, the reaction mixture was analyzed by a gas chromatography, 1,2-dibromotrichloroethane disappeared, and the production of 27.5 g of m-phenoxybenzyl bromide and 20.2 g of m-phenoxybenzylidene dibromide were found.

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; Toyo Soda Manufacturing Co., Ltd.; US4393246; (1983); A;,
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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. 621-23-8, name is 1,3,5-Trimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1,3,5-Trimethoxybenzene

In the reactor, 100 mg of 1,3,5-trimethoxybenzene and 20 mg of boron-nitrogen carbon photocatalyst were added.100 mg of ammonium chloride is an amine source, 3 ml of dimethyl sulfoxide and 1.2 equivalents of cesium fluoride (regulating the pH of the initial reaction solution to 8-10),The reaction was stirred with light at room temperature for 48 h in an oxygen atmosphere, and then extracted with ethyl acetate.The combined organic layers were dried, filtered and evaporatedThe column chromatography eluate used was a petroleum ether: ethyl acetate mixed solvent in a volume ratio of 10:1.The yield was 41%.

According to the analysis of related databases, 621-23-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Fuzhou University; Wang Xinchen; Zheng Meifang; Yuan Tao; Shi Jiale; (7 pag.)CN108546233; (2018); A;,
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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. 532440-88-3, name is 2-Bromo-5-methoxy-4-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 2-Bromo-5-methoxy-4-methylaniline

f. N-(2-bromo-5-methoxy-4-methyl-phenyl)-isobutyramide. To a biphasic mixture of 2-bromo-5-methoxy-4-methyl-aniline (5.6 g, 25.96 mmol), 10% KOH (27 mL) and dichloromethane (30 mL), was added dropwise isobutyryl chloride (3 mL, 28.55 mmol) in dichloromethane (10 mL). The reaction mixture was stirred at room temperature for 48 hrs. The layers were separated. The aqueous layer was further extracted with dichloromethane and the combined organics washed successively with water and brine, dried over MgSO4, filtered and evaporated to give 7.38 g of N-(2-bromo-5-methoxy-4-methyl-phenyl)-isobutyramide (99% yield). 1H NMR (300 MHz; CDCl3): 1.29 (d, J=6.9 Hz, 6 H), 2.14 (s, 3 H), 2.59 (m, 1 H), 3.84 (s, 3 H), 7.24 (s, 1 H), 7.66 (br s, 1 H), 8.07 (s, 1 H).

According to the analysis of related databases, 532440-88-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Pfahl, Magnus; Tachdjian, Catherine; Spruce, Lyle W.; Al-Shamma, Hussien A.; Boudjelal, Mohamed; Fanjul, Andrea N.; Wiemann, Torsten R.; Pleynet, David P.M.; US2003/144329; (2003); A1;,
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