Author: Jessica.F

Application of 1096296-85-3, A common heterocyclic compound, 1096296-85-3, name is (5-Bromo-2-chlorophenyl)methanamine, molecular formula is C7H7BrClN, 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 solution of (5-bromo-2-chloro-phenyl)methanamine (6.5 g, 29.7 mmol) and triethylamine (TEA) (6 g, 59.4 mmol) in CH2CI2 was added methyl chloroformiate (3.35 g, 35.6 mmol) dropwise at 0 C. Then the reaction mixture was stirred at 25C for 10 hours. The reaction mixture was concentrated, diluted with EtOAc(300 mL), washed with brine, and dried over Na2S04. Concentration under reduced pressure gave methyl N-[(5-bromo-2-chloro- phenyl)methyl]carbamate (4 g, yield 49%).

The synthetic route of 1096296-85-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF SE; WINTER, Christian; RHEINHEIMER, Joachim; WOLF, Antje; TERTERYAN, Violeta; POONOTH, Manojkumar; WIEBE, Christine; KREMZOW-GRAW, Doris; ROeHL, Franz; ROHRER, Sebastian Georgios; WIEJA, Andy; ROSENBAUM, Claudia; GRAMMENOS, Wassilios; WO2014/202703; (2014); A1;,
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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. 33863-76-2, name is 1-Bromo-3-chloro-5-fluorobenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-3-chloro-5-fluorobenzene

A mixture of 1-bromo-3-chloro-5-fluorobenzene (8Og, 480mmol), zinc cyanide (33.65g, 290mmol) and zinc dust (0.94g, 14.46mmol) in DMF (34OmL) was stirred at rt for 5 min. Dichloro[1 ,1 ‘- EPO bis(diphenylphosphino)ferrocene] palladium(ll) (4.99g, 16mmol) was then added and the mixture was heated under reflux for 50 min. The reaction mixture was cooled to rt and filtered through Arbocel, washing through with diethyl etherpentane (50:50, 7 x 10OmL). The phases were separated and the organic phase was diluted with water (10OmL) and extracted with further diethyl ethe?pentane (50:50, 3 x 10OmL). The combined organic solutions were then washed with water, dried over magnesium sulfate and concentrated in vacuo. Distillation of the residue under reduced pressure afforded the title compound as a colourless solid in 66% yield, 48.5g. LRMS: m/z APCI 155 [MH+]

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; PFIZER LIMITED; WO2006/67587; (2006); A2;,
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Electric Literature of 13918-92-8, 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 13918-92-8 as follows.

To an ice cooled solution of 5′-amino-7′-nitrospiro[cyclobutane-1,3′-indolin]-2′- one (2.0 g, 8.58 mmol) in DCM (20 mL) were added pyridine (1.4 mL, 17.16 mmol) followed by 2,4-difluorobenzenesulfonyl chloride (1.7 mL, 12.87 mmol) dropwise. The mixture was at RT for 3 h. The mixture was diluted with DCM (100 mL), washed with water (100 mL) and brine (100 mL), dried over sodium sulphate and concentrated under reduced pressure to afford the title compound as yellow solid (2.5 g, 89 %.).1H NMR (400 MHz, DMSO-d6): delta 11.0 (s, 1H), 10.86 (s, 1H), 7.95-7.83 (m, 1H), 7.68 (d, J=1.5 Hz, 1H), 7.62 (d, J=1.5 Hz, 1H), 7.56 (t, J=8.8 Hz, 1H), 7.30-7.25 (m, 1H), 2.47-2.40 (m, 2H), 2.35-2.12 (m, 4H).

According to the analysis of related databases, 13918-92-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ORION CORPORATION; UJJINAMATADA, Ravi Kotrabasaiah; SAMAJDAR, Susanta; ABBINENI, Chandrasekhar; MUKHERJEE, Subhendu; LINNANEN, Tero; WOHLFAHRT, Gerd; (220 pag.)WO2016/203112; (2016); A1;,
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Synthetic Route of 501-29-1, The chemical industry reduces the impact on the environment during synthesis 501-29-1, name is 1-Chloro-2-fluoro-4-methoxybenzene, I believe this compound will play a more active role in future production and life.

4-chloro-3-fluoroanisole (YY-1) in anhydrous THF at -78C under N2(250 mg, 1.56 mmol) was added dropwise a solution of LDA (0.86 mL, 2M,1.71 mmol) and stir for 30 minutes at -78C under N2.DMF (125 mg) was added to the above solution at -78 C under N2.1.71 mmol) and the resulting mixture was stirred at -78 C for 20 minutes.The reaction was quenched with saturated NH4Cl at -78 C. The resulting mixture was heated to 25 C. The mixture was partitioned between EtOAc and H2O.The organic layer was separated and the aqueous layer was extracted with EtOAc. The combined organic layers were washed with brine, dried over Na2SO4 and concentrated to provide the crude product.The crude product is via a flash column (EtOAc: petroleum ether = 1% to 12%)Purified to provide YY-2 (178 mg, 61%) as a white solid.

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-Chloro-2-fluoro-4-methoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PFIZER INC.; KUMPF, ROBERT ARNOLD; MCALPINE, INDRAWAN JAMES; MCTIGUE, MICHELE ANN; PATMAN, RYAN; RUI, EUGENE YUANJIN; TATLOCK, JOHN HOWARD; TRAN-DUBE, MICHELLE BICH; WYTHES, MARTIN JAMES; (445 pag.)TW2018/2074; (2018); A;,
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Electric Literature of 95-51-2, These common heterocyclic compound, 95-51-2, name is 2-Chloroaniline, 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.

(I) in the reaction container by adding O-aminochlorobenzene 0.8mol, aqueous solution 100 ml, control the stirring speed in the 500rpm, by adding the mass fraction is 60% of sodium bromide solution 300 ml, control the temperature of the solution to 9 C, potassium sulfite dropping 0.8mol dissolved in 120 ml of an aqueous solution, keeping the temperature of the solution after the added in 40 C, time-keeping 3h, potassium iodide test for determining the end point of the reaction, the diazonium salt is generated (3);(Ii) taking stannous chloride 0.12mol, the mass fraction of 70% sodium bromide solution of 300 ml mixed in the reaction vessel, heating the solution temperature to 92 C, dropping step (i) generating the diazotizing solution, maintaining the temperature of the solution is in the 95 C, after adding water vapor distillation, oil-free object until the distillate, separating the organic layer, the aqueous layer extracted with ethanol solvent 7 time, combined with the extracted oil, are sequentially used for quality score for the 30 […] 40% phosphoric acid washing, potassium bicarbonate solution, the mass fraction of 10% – 20% of the potassium bromide solution, phosphorus pentoxide dehydration, to extracting distilled 1.3kPa vacuum distillation, collecting 180 – – 185 C fraction, O-chloro-bromobenzene may be colorless transparent product 143.63g, yield 94%.

Statistics shows that 2-Chloroaniline is playing an increasingly important role. we look forward to future research findings about 95-51-2.

Reference:
Patent; Chengdu Railway Technology Co., Ltd. Henghua; Peng, Xiangliang; (4 pag.)CN105541545; (2016); A;,
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These common heterocyclic compound, 698-01-1, name is 2-Chloro-N,N-dimethylaniline, 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-N,N-dimethylaniline

General procedure: To a stirred solution of N,N-dimethylanilines (1, 1.0 mmol) and 2,3-dihydrofuran (2, 10 mmol) in MeCN(20 ml), Co(ClO4)2 (10 mol%) was added. The reactions were performed at 50 C under oxygen atmosphere(O2 balloon) and completed in 48 hours. The products 3 were isolated by flash column chromatographic separation (acetone/petroleum ether = 1:40 to 1:30).

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

Reference:
Article; Huo, Congde; Chen, Fengjuan; Quan, Zhengjun; Dong, Jie; Wang, Yajun; Tetrahedron Letters; vol. 57; 46; (2016); p. 5127 – 5131;,
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Electric Literature of 2267-25-6, The chemical industry reduces the impact on the environment during synthesis 2267-25-6, name is 2-Chloro-4-fluoroanisole, I believe this compound will play a more active role in future production and life.

72-Chloro-4-fluoro-1-methoxybenzene was treated with n-butyllithium and hexachloroethane; the resulting 2,3-dichloro-1-fluoro-4-methoxybenzene was demethylated with boron tribromide to provide the requisite phenol.

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-Chloro-4-fluoroanisole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Pettersson, Martin Youngjin; Johnson, Douglas Scott; Subramanyam, Chakrapani; O’Donnell, Christopher John; Ende, Christopher William Am; Fish, Benjamin Adam; Green, Michael Eric; Mullins, Patrick Bradley; Stiff, Cory Michael; Tran, Tuan Phong; Navaratnam, Thayalan; US2012/252758; (2012); A1;,
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Related Products of 98-60-2, 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. 98-60-2, name is 4-Chlorobenzenesulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To chlorosulfonic acid (10 g, 86 mmol), chlorobenzene(3.23 g,28 mmol) was added dropwise, not to increase temperature over 20C. The solution was stirredat room temperature by 1 hour and it was slowly poured onto ice (50 g). The precipitate wasfiltered off, washed with water and added portionwise to the solution ofnatrium sulfite (7.5 g,60 mmol) in water (28 mL) at temp. 80C.The mixture was stirred at 90Cby 1 hour and 50% natrium hydroxide was slowly dropped to maintain pH= 8-9. Thehot mixture was filtered off and the filtrate was keep at room temperature for10 hours. The white crystals of product 4-chlorobenzenesulfinate natrium saltwas filtered off, washed by cold water and dried at room temperature. Product 3was obtained in 75% yield (4.3 g). IR (cm-1): 1575 (CHar); 1340,1130 (SO2); 1004, 981 (CH); 832, 740 (CCl).

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-Chlorobenzenesulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Staniszewska, Monika; Bondaryk, Ma?gorzata; Ochal, Zbigniew; Bioorganic and Medicinal Chemistry; vol. 23; 2; (2015); p. 314 – 321;,
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Synthetic Route of 50594-82-6, 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. 50594-82-6, name is 3,4,5-Trichlorobenzotrifluoride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(a) Preparation by the process according to the invention 358 g (1.5 mol) of 3,4,5-trichlorobenzotrifluoride were added dropwise to a mixture of 330 g (3 mol) of resorcinol and 111 g (1.5 mol) of calcium hydroxide in 2 liters of dimethylsulfoxide at 120-130 C. in the course of 7 hours. Thereafter, the reaction mixture was stirred at 130 C. for 8 hours. After cooling to room temperature, the reaction mixture was poured into 7 liters of water, whereupon the reaction product separated out as an oil. The mixture was extracted with 3 liters of toluene and the organic phase was separated off and, after drying, was concentrated. The residue was distilled. 350 g (73% of theory) of 2,6-dichloro-4-trifluoromethyl-3′-hydroxydiphenyl ether were obtained in this manner in the form of a solid product of melting point 64-65 C. Boiing point 123-130 C./0.15 mm Hg Analysis: Empirical formula: C13 H7 Cl2 F3 O2: Calculated: 48.3% C; 2.2% H; 22.0% Cl. Found: 48.3% C; 2.3% H; 21.8% Cl.

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, 3,4,5-Trichlorobenzotrifluoride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bayer Aktiengesellschaft; US4264769; (1981); A;,
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Reference of 2267-25-6, 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. 2267-25-6, name is 2-Chloro-4-fluoroanisole belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2-chloro-4-fluoroanisole (38g, 237mmol) concentrated sulfuric acid (100mL) solution, bromine (19mL, 737mmol) was added under ice-cooling, and the mixture was stirred for 1.5 hours. It was added to the reaction solution gradually into ice water, and extracted with diethyl ether (300mL ¡Á 3). After washing the organic layer with 5% aqueous sodium thiosulfate solution (300 mL), the organic layer was dried over anhydrous magnesium sulfate, filtered, and the crude product obtained through concentration under reduced pressure by silica gel chromatography – (hexane: ethyl acetate = 1 : 0 to 10: 1) to give 5-bromo-2-chloro-4-fluoroanisole of a white solid (8.0g, yield: 14%) and 2-bromo-6-chloro-4-fluoroanisole of a white solid (16.7g, yield: 30%)It was obtained.

The synthetic route of 2-Chloro-4-fluoroanisole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SAGAMI CHEMICAL RESEARCH INSTITUTE; KAKEN PHARMACEUTICAL COMPANY LIMITED; KOBAYASHI, OSAMU; TAKATSUNA, REIKO; NIIKURA, NAOKO; TATENO, TOMOKO; NAKAMURA, SHINJI; HIRAI, KENJI; KOCHI, SHINICHIRO; KAWANISHI, NAOKI; YAMADA, OSAMU; (76 pag.)JP2016/60742; (2016); A;,
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