Category: 19752-55-7

19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, 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. SDS of cas: 19752-55-7

Magnesium turning (2.8 g) and iodine (50 mg) were added to a 250 mL three-necked round bottom flask and stirred under an argon atmosphere for 30 minutes. 1-bromo-3,5-dichlorobenzene (20.7 g) dissolved in tetrahydrofuran was slowly added dropwise, heated to reflux for 2 hours, and then cooled to room temperature. In another round bottom flask, trimethoxyboraine (33.8 mL) was dissolved in 80 mL of diethyl ether. After cooling to -15 C, a previously prepared Grignard reagent was added dropwise through a cannula. Slowly raised to room temperature and stirred for 12 hours. The resulting white solid was washed with pentane and the filtrate was concentrated under reduced pressure to give 14.6 g of the title compound.

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

Reference:
Patent; Dae Joo Electronic Materials Co., Ltd.; Jeon Yeong-min; Park Jeong-gyu; Lee Hyeon-seok; Kim Min-yeong; (50 pag.)KR2019/106313; (2019); A;,
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Synthetic Route of 19752-55-7, A common heterocyclic compound, 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, molecular formula is C6H3BrCl2, 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.

In Nitrogen environment I-16(99 g, 208 mmol) was dissolved in in 600 mL tetrahydrofuran (THF), where the 1-bromo-3,5-dichlorobenzene(56.4 g, 250 mmol) and tetrakis( triphenylphosphine) palladium was stirred into the (2.40 g, 2.08 mmol) into a saturated potassium carbonate in water (71.9 g, 520 mmol) was heated to reflux at 80 ° C for 8 hours. After the reaction was completed, the reaction solution into water and extracted with dichloromethane (DCM) and then water was removed with anhydrous MgSO4, filter and was concentrated under reduced pressure. Thus the resulting residue was separated and purified by flash column chromatography to obtain the compound I-17(53.7 g, 79percent).

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

Reference:
Patent; Cheil Industries Co., Ltd; Lee, Han Ir; Yu, Uhn Sun; Kang, Dong Min; Kang, Uii Soo; Yang, Yong Tak; Oh, Jae Jin; Yu, Dong Gyu; Lee, Sang Sin; Jang, Yuna; Jung, Su Young; Han, Su Jin; Hong, Jin Suk; (59 pag.)KR2015/6758; (2015); 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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C6H3BrCl2

Example 2; Step 1; Magnesium turnings (5.38 g) and THF (50 ml) were placed in a dry flask equipped with a dropping funnel which contained a mixture of 1-bromo-3,5-dichiorobenzene (50 g) and THF (300 ml). 30 Milliliters of the solution in the dropping funnel was added to the flask. A few drops of dibromoethane were added to he flask to help initiate the reaction. After a few minutes, solvent in the reaction flask started to boil. The remaining solution in the dropping funnel was added drop wise. Ice water was used occasionally to coo. the reaction mixture. After the addition, the mixture was stirred at room temperature for two hours. Benzonitriie (22,82 g) was added to the reaction mixture. The mixture was refiuxed for 2 days. 3 N HC1 (300 mL} was added, The mixture was stirred for 4 hours and extracted using ethyl acetate. The organic layer was collected in a separatory funnel and concentrated. The obtained oil (49 g) was used in the next step without further purification.

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

Reference:
Patent; TRANSITIONS OPTICAL, INC.; WO2012/82506; (2012); A1;,
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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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 19752-55-7

To a solution of 1-bromo-3,5-dichlorobenzene (25.0 g, 1 10.6 mmol) in 400 ml THF at room temperature, isopropyl magnesium chloride lithium chloride complex (85.0 ml, 1.3M THF, 1 10.6 mmol) was added dropwise at room temperature over a period of 15 minutes while holding the reaction temperature between 20°C and 25°C. After the addition was complete, the reaction was allowed to stir 1.5 hours at room temperature. The reaction solution was then cooled to -5 °C to -10 °C with ice/MeOH. Methyltrifluoroacetate (12.23 ml, 121 .6 mmol) in 20 ml THF was added dropwise to the reaction solution while maintaining the reaction temp below 0 °C (~ 30 min). The reaction was stirred at -5 °C for 0.5 hr then was allowed to warm to room temperature and stir for 1.5 hrs. The reaction was cooled again to -5 °C to -10 °C then 73.7 ml 6M HCI diluted to 150 ml total volume water was added dropwise while keeping the temperature below 0 °C. Once the addition was complete, the reaction was stirred 0.5 hr at 0 °C then was allowed to warm to room temperature. Excess water was added and the resulting organic layer that separated was drawn off. The aqueous layer was washed repeatedly with DCM. The combined DCM washes and recovered organic layer were dried over sodium sulfate and concentrated to yield 90 g of an oil. The crude material was then passed through a silica gel plug (neat heptane to neat DCM) and purified by vacuum distillation (3 torr, product fractions recovered froml 12 °C to 125 °C) to provide 20.3 g product (75.7percent yield). 1 H NMR (400 MHz, CHLOROFORM-d) delta ppm 7.71 (s, 1 H) 7.93 (s, 2 H). IR 1728.1 cm”1

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 19752-55-7.

Reference:
Patent; AVISTA PHARMA SOLUTIONS, INC.; SPEAKE, Jason, D.; (57 pag.)WO2018/9751; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C6H3BrCl2

Under a nitrogen atmosphere, tert-butyllithium (1.3 Msolution in Pentane, 17.8 mL, 23.2 mmol) was added dropwise to a solution of 3,5-dichlorobenzene (5.0 g, 22.1mmol) in tetrahydrofuran (50 mL) for 30 min and the reaction was continued for 2 hours. Trifluoroacetic anhydride is then added(2.56 g, 12.2 mmol) was added dropwise to the mixed solution and stirring was continued for 2 hours while maintaining at -78 ° C. Remove the cold, gradually rose toAfter room temperature, keep the reaction at room temperature for 2.5 hours. Saturated ammonium chloride solution (50 mL) was added to terminate the reaction. The mixture was extracted with etherThe organic phase was combined and washed with saturated brine (20 mL’2). The organic phase was separated and washed with anhydrous magnesium sulfateDrying, filtration, removal of the solvent, and distillation under reduced pressure gave a colorless transparent liquid 1 (2.58 g) in a yield of 48percent.

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

Reference:
Patent; Jingmen Pharmaceutical Industry Technology Institute; Wang Yong; Li Liwei; Hu Jianmei; Gu Dongyun; Huang Daoyou; (12 pag.)CN107353189; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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

EXAMPLE 3 In the reactor of Example 1, each chlorination of 1-bromo-3,5-dichlorobenzene was chlorinated under the specific condition. The starting materials were respectively preheated at 300 C. and 1-bromo-3,5-dichlorobenzene was fed at a rate of 7.7 g./min. and chlorine was fed at a rate of 550 ml./min. into the reactor. The reaction was continuously carried out at a reaction temperature of 360 C. and a residence time of 14 seconds for 2 hours. The reaction mixture was cooled to collect 1029 g. of the mixture. The reaction mixture was distilled to recover 263 g. of bromine (recovery percent of 84%). The residue contained the object product and a small amount of bromine and it was washed in an aqueous solution of sodium thiosulfate and the product was separated under heating it by a phase separation to obtain 722.5 g. of 1,3,5-trichlorobenzene as the object product (yield of 97.2%).

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; Ishihara Sangyo Kaisha Ltd.; US4368340; (1983); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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

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

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.

To 5.1 g (0.209 mol) of magnesium turnings were added 0.45 g of a 1 molar solution of DIBAL in hexane at 60°C. After 15 min, 3,5-dichloro-bromobenzene (5.0 g, 0.022 mol) and 25 mL THF were added and the mixture was stirred. After start up of the reaction a mixture of 45g (0.2 mol) 3,5-dichloro-bromobenzene and 250 mL THF was added under reflux. After completion of the reaction the mixture was cooled to 0°C and 31 .1 g (0.219 mol) of ethyl trifluoroacetate were added. After 2 h an aqueous solution of NH4CI was added and the mixture was separated between MTBE and aqueous N H4CI solution. The organic layer was separated and the solvent was removed in vacuum. (34.3g brown oil; purity 70percent acc. to g.c; yield 50percent)1H-NMR (360 MHz, CDCI3): delta = 7.7 (s, 1 H), 7.9 (s, 2H) ppm.

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

Reference:
Patent; BASF SE; KOeRBER, Karsten; KORDES, Markus; RACK, Michael; VON DEYN, Wolfgang; KAISER, Florian; WO2012/59441; (2012); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 19752-55-7, 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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: 3,5-Dichloro-1-bromobenzene (7.46 g, 33.0 mmol) or 3,5-bis(trifluoromethyl)-1-bromobenzene (9.67 g, 33.0 mmol) was dissolved in ether (70 mL). To this solution, BuLi (1.58 M in hexane, 20.9 mL, 33.0 mmol) was added using syringe through septum cap at -78 °C for 20 min, and the mixture was stirred for 2 h at -78 °C. To the reaction mixture a solution of antimony (III) boromide (3.61 g, 10.0 mmol) in ether (50 mL) was added dropwise at -78 °C, and the resulting mixture was gradually raised to room temperature and stirred overnight. The reaction mixture was diluted with ether (150 mL) quenched with water. The mixture was extracted with ether (150 mL). The combined extracts were washed with brine and dried over anhydrous magnesium sulfate. The dried organic layer was concentrated under reduced pressure. The residue was purified on silica gel column chromatography to give 1n (hexane, 4.5 g, 80 percent yield) and 1o (hexane: CH2Cl2 4:1, 6.9 g, 91 percent yield).

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

Reference:
Article; Yasuike, Shuji; Nakata, Kazuhide; Qin, Weiwei; Matsumura, Mio; Kakusawa, Naoki; Kurita, Jyoji; Journal of Organometallic Chemistry; vol. 788; (2015); p. 9 – 16;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics