Month: May 2021

Reference of 25186-47-4, A common heterocyclic compound, 25186-47-4, name is 3,5-Dichlorotoluene, molecular formula is C7H6Cl2, 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.

To a stirred solution of l ,3-dichloro-5-methylbenzene (2.0 g, 12.4 mmol) in THF (20 mL) was added n-BuLi (2.0 M in hexane, 9.3 mL, 18.6 mmol) at -78 C dropwise over a period of 10 miri and mixture was stirred at -78 C for 30 min. A dry-ice was added to the reaction mixture slowly and the mixture was stirred at the same temperature for 20 min. Thereafter, the reaction mixture was slowly warmed to room temperature, quenched with 6 M HC1 (10 mL) and extracted with EtOAc (2 x 30 mL). The combined organic layers were washed with water (50 mL), brine (50 mL), dried over anhydrous Na2S04 and concentrated under reduced pressure to get compound Al 11 -1 (1.1 g, 44%) as a white solid.

The synthetic route of 25186-47-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TEIJIN PHARMA LIMITED; AMGEN INC.; BECK, Hilary Plake; BOOKER, Shon Keith; BREGMAN, Howard; CEE, Victor J.; CHAKKA, Nagasree; CUSHING, Timothy D.; EPSTEIN, Oleg; FOX, Brian M.; GEUNS-MEYER, Stephanie; HAO, Xiaolin; HIBIYA, Kenta; HIRATA, Jun; HUA, Zihao; HUMAN, Jason; KAKUDA, Shinji; LOPEZ, Patricia; NAKAJIMA, Ryota; OKADA, Kazuhisa; OLSON, Steven H.; OONO, Hiroyuki; PENNINGTON, Lewis D.; SASAKI, Kosuke; SHIMADA, Keiko; SHIN, Youngsook; WHITE, Ryan D.; WURZ, Ryan P.; YI, Shuyan; ZHENG, Xiao Mei; WO2015/129926; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 7051-15-2, name is 2-Chloro-1,3-dimethoxybenzene, 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. Recommanded Product: 2-Chloro-1,3-dimethoxybenzene

The 13.9g acetophenone (115.6mmol), 10.9g chlorobenzene (96.7mmol), 11.1g sodium tert-butoxide (115.6mmol) and 0.35g azacarbene imine palladium catalyst added in Example 6 9.8g p-cyanoacetophenone (67.3mmol), 9.6g 2,6-dimethoxychlorobenzene (56.1mmol), 6.5g sodium tert-butoxide (60mmol) and 0.2g azacyclocarbene imines The palladium catalyst and 60 mL of 1,4-dioxane solvent were not changed under other conditions, and the target product was obtained 14.0 g, and the isolated yield was 89%.In Example 6, the 0.35g nitrogen heterocyclic carbene imine palladium catalyst A1 was replaced with 0.24g A2, 0.29g A3, 0.34g A4, 0.24g A5, and the separation yields were 98%, 96%, 90%, 90%.

The synthetic route of 2-Chloro-1,3-dimethoxybenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Chemical Institute Co., Ltd.; Lu Huiyang; Shen An; Cao Yucai; Li Yongqing; Ni Chen; Hu Yucai; (14 pag.)CN110818545; (2020); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 21402-26-6, 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. 21402-26-6, name is 4-Bromo-3-chloroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 1 Preparation of N,N-Dipentyl-4-bromo-3-chloroaniline (1). 1-Bromopentane (0.42 mL, 3.4 mmol) was added to a mixture of 4-bromo-3-chloroaniline (200 mg, 0.9 mmol) and potassium carbonate (199 mg, 1.4 mmol) in DMF (20 mL) and the reaction was heated to 13 0~~C overnight. The mixture was cooled, diluted with water (20 mL) and extracted with petroleum ether (3*25mL). The combined organic extracts were dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified via flash column chromatography using 9:1 petroleum ether:ethyl acetate as eluent to give N,N-Dipentyl-4-bromo-3-chloroaniline (1) (332 mg, 68%). 1H-NMR (CDCI3) 67.02 (d, IH, ArH); 3.12 (t, 4H, 2*NCH2); 0.95 (t, 6H, 2*CH3). MS; 347 (M+H).

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

Reference:
Patent; Oxford Glycosciences (UK) Ltd.; US6262263; (2001); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 320-50-3, name is 1,4-Dichloro-2-(trifluoromethyl)benzene, belongs to chlorides-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 320-50-3, Quality Control of 1,4-Dichloro-2-(trifluoromethyl)benzene

Similarly, 4-(2-trifluoromethyl-4-chlorophenoxy)benzene is prepared by following the same procedure but using 1,4-dichloro-2-trifluoromethylbenzene in place of 1,2-dichloro-4-trifluoromethylbenzene.

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, 1,4-Dichloro-2-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Chevron Research Company; US4287213; (1981); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 102170-53-6, name is 4-Bromo-5-chloro-2-methoxyaniline, A new synthetic method of this compound is introduced below., SDS of cas: 102170-53-6

Intermediate 7: 2-Amino-5-bromo-4-chlorophenol 4-Bromo-5-chloro-2-methoxyaniline (Intermediate 6, 10g, 42.3 mmol) in DCM (200 mL) was cooled to 0 C. Boron tribromide (21 .2 g, 84.6 mmol) was added drop-wise over 30 min, the reaction mixture was stirred at 0 C for 1 h and then at room temperature for 14 h. The reaction mixture was poured into ice water, sodium hydrogen carbonate was added until pH >7 and aqueous layer was extracted with ethyl acetate (300 mL x 3). The organic phase was dried over magnesium sulphate and the solvent removed under vacuum to give 2-amino-5-bromo-4-chlorophenol as a red solid (8.4 g, 89%, used without further purification for the next step). LCMS (A): Rt 1.46 min, MH+ 222/224.

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; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; BOUILLOT, Anne Marie Jeanne; MIRGUET, Olivier; LIDDLE, John; WALKER, Ann, Louise; WO2015/91647; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 928-50-7 as follows. Product Details of 928-50-7

Equipped with a mechanical stirrer, a reflux condenser and a thermometer 1000ml four-necked flask, followed by adding 50g (0.48mol) 5- chloro-1-pentene, 50g (0.27mol) phthalimide potassium salt, triphenyl phosphine bromide 0.25g, 2.5g and 500g of nickel sulfate, hexamethylphosphoric triamide. After the addition was complete, the oil bath was heated to 200 deg.] C, the reaction was kept for 3 hours. After incubation, cooled to room temperature. Filter cake by-product potassium chloride reactions, polymerization inhibitor and a catalyst. Rinsed with acetone 100ml fresh cake combined filtrate and washings. Under reduced pressure using a rotary evaporator, acetone was distilled off spin, hexamethylphosphoric triamide and the excess of 5-chloro-1-pentene. Get 57g red viscous liquid, liquid chromatography measured content of 94.81%, the yield was 98.09%.

According to the analysis of related databases, 928-50-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Yizheng Haifan Chemical Co., Ltd; Zou, Congwei; (9 pag.)CN106008314; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 202865-57-4, name is 1-Bromo-2,5-dichloro-3-fluorobenzene, 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. Formula: C6H2BrCl2F

To a solution of potassium KO’Bu (20.7 g, 185 mmol)) suspended in toluene (270mL) and DMPU (90 mL, 746 mmol) was added methanol (30 mL). The mixture was placed in an oil bath at 80 C under N2 with a reflux condenser for 25 minutes to obtain a solution. The solution was then allowed to cool to room temperature under N2, after which l-bromo-2,5-dichloro-3- fluorobenzene (15 g, 61.5 mmol) was added dropwise to the solution and the resulting suspension was placed in an oil bath at 80 C under N2. After 4 h, the reaction mixture was allowed to cool to room temperature and was then diluted with hexanes (200 mL) and water. The layers were separated and the aqueous layer was extracted with hexanes. The combined organic portions were washed with water, dried (MgS04), filtered and concentrated to afford crude. The crude was purified by silica gel chromatography using 30% EtOAc/pet ether as an eluent to afford l-bromo-2,5-dichloro-3-methoxybenzene (13 g, 81% yield) as off white solid. 1 H NMR (300 MHz, CDCL) d 7.26 (d, J = 2.8 Hz, 1H), 6.87 (d, J = 2.8 Hz, 1H), 3.93 (s, 3H).

The synthetic route of 1-Bromo-2,5-dichloro-3-fluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; BANDYOPADHYAY, Anish; CHEUNG, Mui; EIDAM, Hilary Schenck; JOSHI, Hemant; SU, Dai-Shi; (128 pag.)WO2019/149959; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 1000577-58-1, These common heterocyclic compound, 1000577-58-1, name is 1-Bromo-2,3-dichloro-5-fluorobenzene, 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.

Synthesis of 1-bromo-2.3-dichloro-5-methoxybenzene (Compound 2)[0151] 1-Bromo-2,3-dichloro-5-fluorobenzene (5.1453 g, 21.10 mmol) was dissolved in THF (25 mL) at room temperature and cooled to 0 C. Then, 5.1 g of sodium hydride (60%, 128 mmol) was added and 2.0 mL of methanol was added slowly. Additional THF (5 mL) was added. The mixture was stirred at room temperature for 10 minutes, then heated at 75 C for four hours and cooled to room temperature. The mixture was poured into ice with some aq. sat. NH4Cl solution and extracted with EtOAc (3 x 100 mL). The organic solution was washed with brine, dried over Na2SO4, concentrated to dryness. The residue was purified with flash column chromatography on silica gel using hexane as solvent to afford the product (4.6727 g) as a white solid in 87% yield. 1H-NMR (CDCl3): delta 7.109 (d, J = 3.0 Hz, 1 H), 6.988 (d, J- 3.0 Hz, 1 H), 3.786 (s, 3 H). The product was also synthesized from l-bromo-2,3-dichloro-5-fluorobenzene and sodium methoxide in THF. The final product was purified by recrystallization from hexane.

Statistics shows that 1-Bromo-2,3-dichloro-5-fluorobenzene is playing an increasingly important role. we look forward to future research findings about 1000577-58-1.

Reference:
Patent; NEKTAR THERAPEUTICS; RIGGS-SAUTHIER, Jennifer; DENG, Bo-Liang; WO2010/132691; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2162-98-3, name is 1,10-Dichlorodecane, belongs to chlorides-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 2162-98-3, Product Details of 2162-98-3

Example 1 20.6 g (0.1 mol) of 4-octylaminopyridine, 10.5 g (0.05 mol) of 1,10-dichlorodecane and 30 ml of demineralized water were combined and refluxed with stirring. The initially cloudy, yellowish solution became clear and yellow after 3 hours. After the mass had been stirred for a further hour at reflux, it was cooled to 5 C. The resulting white, semisolid paste was filtered off with suction, and the product octenidine dihydrochloride in the form of colourless crystals was washed with iced water.

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, 1,10-Dichlorodecane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; AIR LIQUIDE SANTE (INTERNATIONAL); US2001/16660; (2001); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 454-78-4, 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. 454-78-4, name is 2-Bromo-1-chloro-4-(trifluoromethyl)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of l-(3,4-dihydroisoquinolin-2(lH)-yl)-3-(3-(4,4,5,5-tetramethyl- 1,3,2- dioxaborolan-2-yl)phenoxy)propan-2-ol (200 mg, 0.489 mmol), 2-bromo-l- chloro-4- (trifluoromethyl)benzene (126 mg, 0,489 mmol), Pd(dppf)Cl2 (36 mg, 0.049 mmol), K2C03 (202 mg, 1.47 mmol) in H20-dioxane (1 mL/ 3 mL) was stirred at 100C under microwave heating for 15 min. The solvent was removed and the crude product purified by HPLC separation to give the title compound as the TFA salt (186 mg, 85%) 1HNMR (CH3OD, 400MHz) delta: 7.76-7.63 (m, 3H), 7.46-7.40 (m, 1H), 7.38-7.20 (m, 4H), 7.11-7.02 (m, 3H), 4.78-4.40 (m, 3H), 4.18-4.08 (m, 2H), 4.02-3.84 (m, 1H), 3.67-3.40 (m, 3H), 3.38-3.16 (m, 2H). LCMS (m/z): 462.2 [M+H]+

The synthetic route of 2-Bromo-1-chloro-4-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EPIZYME, INC.; DUNCAN, Kenneth, W.; CHESWORTH, Richard; MUNCHHOF, Michael, John; JIN, Lei; WO2014/100695; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics