Month: August 2021

Electric Literature of 19752-55-7,Some common heterocyclic compound, 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, molecular formula is C6H3BrCl2, 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.

Intermediate 1-2 (6.0 g, 0.018 mol) in intermediate 1-3 (3.3 g, 0.008 mol), Pd (pph3) 4 (1.0 g, 0.0009 mol), potassium carbonate (6.5 g, 0.036 mol) in THF 130 mL of insert was reacted with stirring for 4 hours at 65 °C. After the end of the reaction H2O: column purification after determination in MC (n-HEXANE: MC) to compound 1 to afford 9.3 g (71percent). Intermediate 1-2 (6.0 g, 0.018 mol) in 1-bromo-3 ,5-dichlorobenzene (1.8 g, 0.008 mol) into the Example 1-Preparation Example 4 in the same manner used in the synthesis to give the 3.1 g (yield 73percent)

The synthetic route of 19752-55-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; P&H Tech; Hyeon, Seo Young; Chong, Song Wook; Kim, Dong Won; (52 pag.)KR2015/137265; (2015); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 13526-66-4, name is 3-Bromo-6-chloroimidazo[1,2-b]pyridazine, 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: 3-Bromo-6-chloroimidazo[1,2-b]pyridazine

In an inert atmosphere, 506 mg (2.2 mmol) of intermediate 1 , 1 g (2.3 mmol) of the crude 2-stannylbenzofurane, 41 mg (0.22 mmol) copper (.) iodide and 76 mg (0.1 1 mmol) bis(triphenylphosphine) palladium(ll)chloride in 18 mL of THF is stirred over night at 85 C in a sealed pressure tube. The solvent was evaporated, the obtained solid was digested in methanol and filtered off. The solid remainder was subjected to flash chromatography to yield 282 mg (39%) of the title compound as solid material. 1H-NMR (400 MHz, DMSO-d6), delta [ppm]= 3.99 (3H), 7.02 (1 H), 7.23 (1 H), 7.35 (1 H), 7.55 (1 H), 7.62 (1 H), 8.37-8.43 (6H).LCMS (Method 1 ): R, = 1 .29 min; MS (ESIpos) m/z = 300 [ +H]

The synthetic route of 3-Bromo-6-chloroimidazo[1,2-b]pyridazine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER INTELLECTUAL PROPERTY GMBH; KNUT, Eis; PUeHLER, Florian; ZORN, Ludwig; SCHOLZ, Arne; LIENAU, Philip; GNOTH, Mark; BOeMER, Ulf; GUeNTHER, Judith; FANGHAeNEL, Joerg; KORR, Daniel; WO2012/163942; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 6579-54-0, 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. 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 18 2,6-dichloro-N-[(3R)-1-cyano-3-pyrrolidinyl]benzenesulfonamide To a chilled (0 C.) solution of 1,1-dimethylethyl (3R)-3-amino-1-pyrrolidinecarboxylate (0.085 ml, 0.0501 mmol) in THF (1 ml) was added triethylamine (0.275 ml, 1.97 mmol) and 2,6-dichlorobenzenesulfonyl chloride (0.1235 g, 0.50 mmol). The reaction mixture was stirred at room temperature overnight, then diluted with water, extracted with DCM and concentrated. To the residue was added 4N HCl in 1,4-dioxane (3.0 ml). After stirring at room temperature overnight, the solvent was evaporated, the residue diluted with DCM (10 ml), and mixed with DIEA (0.2 mL, 1.15 mmol) and BrCN (0.40 mL, 1.2 mmol). The resultant mixture was stirred at room temperature overnight. The solvent was evaporated under vacuum and the solid purified by preparatory HPLC (without TFA) to afford the title compound (0.0412 g). LC-MS: m/z, 320 (M+H), rt 1.66 min.

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, 2,6-Dichlorobenzenesulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DENG, Jianghe; Laine, Dramane Ibrahim; McCleland, Brent W.; Palovich, Michael R.; Petitjean, Emilie Veronique; US2009/264499; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 202925-07-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 202925-07-3 name is 2-Chloro-1-fluoro-4-methoxybenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Example 47; (2-Amino-6-chloro-pyridin-3-yl)-(4-chloro-5-fluoro-2-methoxy-phenyl)-methanone; A. 5-Chloro-4-fluoro-2-iodoanisole; To a solution of 3-chloro-4-fluoroanisole (4.69 g, Lancaster) in chloroform (250 mL) was added silver trifluoroacetate (23.2 g, Aldrich) followed by iodine (15.8 g, Aldrich) in several portions. The reaction mixture was stirred for 2 hours and filtered through Celite. The filtrate was washed with water, brine, dried and concentrated. The crude product was purified by crystallization from ether/petroleum ether to give 5-chloro-4-fluoro-2-iodoanisole (5.0 g). MS (M+H)+, 285.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-1-fluoro-4-methoxybenzene, and friends who are interested can also refer to it.

Reference:
Patent; Bartkovitz, David Joseph; Chu, Xin-Jie; Lovey, Allen John; Wovkulich, Peter Michael; US2006/14708; (2006); A1;,
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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, A new synthetic method of this compound is introduced below., Product Details of 19752-55-7

Xphos 42.80mg, at the same time added to a dry 25ml eggplant, and dissolved with toluene, stir. among them,The catalyst was 2.5percent mol of reactant 1 and the ligand was 10percent mol of reactant 1; the catalyst and ligand MoThe ratio is 1: 4.Next, 205.4 mg of 3,5-dichloro-1-bromobenzene (Reactant 1) was added to the bottle at 35 ° C,Continue stirring 3min. Then, 293.95 mg of tris (trimethylsilyl) yttrium (reactant 2) was dissolved with toluene,To obtain a concentration of 0.5mol / L solution, and the solution was added dropwise to the reaction solution by syringe, dropping timeFor 1h. After the addition was completed, continue to react 1h. Among them, tris (trimethylsilyl) yttrium and 3,5-dichloro-1-Bromobenzene molar ratio of 2: 5.Finally, the product was isolated and purified by column chromatography to give the product as a yellow liquid1- (trimethylsilyl)Methyl) -3,5-dichlorobenzene 6A, mass 152.68 mg, 72percent yield, conversion up to 100percent. among themThe eluant used for the column chromatography was a mixed solution of petroleum ether and ethyl acetate, and the molar ratio of petroleum ether and ethyl acetateThe ratio is 1: 0.1.

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; Beijing Institute of Technology; Li Xiaofang; Cai Guilong; Zhou Yuening; He Jianyun; Huang Yingda; (37 pag.)CN104496736; (2016); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 2106-02-7, These common heterocyclic compound, 2106-02-7, name is 2-Chloro-4-fluoroaniline, 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: The aniline (1 eq, 0.0017 mol) was added to amixture of 5 (0.5g, 0.0017 mol), ethanol: water (7:3mL) and 4-5 drops of HCl (pH is 5-6). The reactionmixture was stirred for 4 hr at 65-70 0 . The reactionmixture was cooled to RT, a solid separated out whichwas filtered, washed with water (10 mL) and dried.The crude product was purified by recrystallizationfrom ethanol-water (2:1) to obtain pure 6.

The synthetic route of 2106-02-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Rajitha, Ch.; Vineel, B. George; Venkataiah; Dubey; Indian Journal of Heterocyclic Chemistry; vol. 24; 3; (2015); p. 325 – 328;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

104-11-0, name is 1-(4-Chlorophenyl)-N-methylmethanamine, belongs to chlorides-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. Safety of 1-(4-Chlorophenyl)-N-methylmethanamine

General procedure: N,N?-dimethyl-1,1?-binaphthyl-2,2?-diamine (1) (1 eq, 3.20 mmol, 1.0 g) and Et3N (3 eq, 9.6 mmol, 1.33 mL)were dissolved in dry THF (32 mL). The homogeneous mixture was cooled to 0 C then PCl3 (3 eq, 9.60 mmol,0.84 mL) was added dropwise via syringe whereupon a colorless precipitate formed immediately. Thereaction mixture was stirred at 0 C for 1.5 h, then was allowed to warm to room temperature and stirred foranother 3 h. The volatiles were removed under high vacuum (room temperature, 0.5mmHg) and Et2O (30.0mL) was added via syringe, then the mixture was stirred for 5 min. After that the supernatant was canulafilteredinto another round bottom flask. The remaining precipitate in the reaction flask was washed againwith Et2O (30 mL) and filtered (2 times). The volatiles were removed under high vacuum (room temperature,0.5 mmHg) to afford a light yellow solid. The solid was then dried for 12 h at reduced pressure (roomtemperature, 0.5 mmHg) to give a white solid foam (2). Dry CH2Cl2 (40 mL) was added via syringe and themixture was cooled to 0 C. To this solution, a mixture of Et3N (2 eq, 6.40 mmol, 0.98 mL) and the desiredmethylamine (3) (1.2 eq, 3.84 mmol) dissolved in dry CH2Cl2 (4 mL) were added. The reaction mixture was allowed to warm to room temperature and stirred for 20 h. A solution of mCPBA (70%) (1.5 eq, 4.80 mmol,1.18 g) dissolved in 2 mL of THF was then added and the mixture was stirred for 20 h. After a quench with 15mL of NH4Cl saturated aqueous solution, the phases were separated and aqueous layer was washed withCH2Cl2 (10 mL). The combined organic extracts were washed with brine, dried over Na2SO4, filtered andconcentrated by rotary evaporation. The crude residue was purified by silica gel flash chromatography usingethyl acetate (100%) as eluent to yield phosphoroamides with different yields.

The synthetic route of 104-11-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Rossi, Sergio; Ziliani, Marco; Annunziata, Rita; Benaglia, Maurizio; Molecules; vol. 22; 12; (2017);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 210532-25-5, name is 3,5-Difluorobenzene-1-sulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3,5-Difluorobenzene-1-sulfonyl chloride

General procedure: To a solution of intermediate 13 (10mmol) and triethylamine (15mmol) in dichloromethane (20ml), a solution of appropriate acyl chlorides or sulfonyl chlorides (1.05 eq) in dichloromethane (3ml) was added dropwise at room temperature overnight. The mixture was washed with saturated aqueous sodium bicarbonate and brine. After removing the solvent under reduced pressure, the crude product was purified by flash chromatography on silica gel to yield the intermediates 14a-n, 15a-k, 16a-h, 17a-m. Subsequently, to a solution of the above intermediates (2mmol) in methanol/H2O (75%, 10ml) was added lithium hydrate (2.4mmol). The resulting mixture was allowed to warm up to 60C for 4h. The reaction mixture was allowed to cool to room temperature and concentrated under pressure to remove methanol. The resulting mixture was diluted by water and acidified with aqueous HCl (1mol/L) till pH=3. The white solid was collected by filtration, washed with water three times and dried to give the target compounds.

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 210532-25-5.

Reference:
Article; Guo, Yongzhi; Zhao, Yuqian; Wang, Guan; Chen, Yi; Jiang, Yingnan; Ouyang, Liang; Liu, Bo; European Journal of Medicinal Chemistry; vol. 143; (2018); p. 402 – 418;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, 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 1871-57-4, SDS of cas: 1871-57-4

General procedure: To a cooled solution (5 C) of the corresponding 4,6-O-(R)-benzylidene-d-hexopyranoside derivative (obtained using the procedure describe by our group2c) (35.4 mmol) in dry THF (70 mL) were added, successively, freshly powdered potassium hydroxide (7.0 g, 125 mmol), 18-crown-6 (0.38 g, 1.4 mmol), and 3-chloro-2-chloromethylpropene (4.1 mL, 35.4 mmol). The reaction mixture was stirred at this temperature for 3 h, and left at room temperature until all the starting material had been consumed, as monitored by TLC (5-7 days, approximately), then diluted with dichloromethane (60 mL) and washed successively with water and aqueous saturated solution of sodium bicarbonate, dried (MgSO4), filtered, and the filtrate was evaporated to dryness.

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:
Article; Vega-Perez, Jose M.; Vega-Holm, Margarita; Perinan, Ignacio; Palo-Nieto, Carlos; Iglesias-Guerra, Fernando; Tetrahedron; vol. 67; 2; (2011); p. 364 – 372;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 57946-56-2, These common heterocyclic compound, 57946-56-2, name is 4-Chloro-2-fluoroaniline, 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.

The starting material was prepared as follows: A solution of 7-benzyloxy-4chloro-6-methoxyquinazoline (1.2 g, 4 mmol), (prepared as described for the starting material in Example 1), and 4-chloro-2-fluoroaniline (4441 mul, 4 mmol) in 2-propanol (40 ml) was refluxed for 1.5 hours. After cooling, the precipitate was collected by filtration, washed with 2-propanol then ether and dried under vacuum to give 7-benzyloxy-4-(4-chloro-2-fluoroanilino)-6-methoxyquinazoline hydrochloride (1.13 g, 64%). m.p. 239-242 C. 1H NMR Spectrum: (DMSOd6) 4.0(s, 3H); 5.36(s, 2H); 7.39-7.52(m, 9H); 8.1(s, 1H); 8.75(s, 1H); MS-ESI: 410 [MH]+; Elemental analysis: Found C, 59.2; H, 4.3; N, 9.4; C22H17N3O2ClF 1 HCl Requires C, 59.2; H, 4.1; N, 9.41%.

Statistics shows that 4-Chloro-2-fluoroaniline is playing an increasingly important role. we look forward to future research findings about 57946-56-2.

Reference:
Patent; Zeneca Limited; Zeneca Pharma S.A.; US6414148; (2002); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics