Category: bromides-buliding-blocks

Related Products of 38573-88-5, 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 38573-88-5 as follows.

Isopropylmagnesiumchloride-LiCl complex (1,30 M in THF, 155.0 mL, 0.0715 mol) under nitrogen was cooled to 0-5 ¡ãC, and 2,3-difluorobromobenzene (13.8 g, 0.0715 mol, 1.50 equiv.) was added while T < 10 ¡ãC. After 1 h at 0-5 ¡ãC, a solution of 1 -morpholino-2-( 1 -(trityloxy)but-3-en-2-yloxy)ethanone 14 (21.8 g, 0.048 mol, 1.0 equiv.) in THF (2.0 vols) was added while T <10 ¡ãC. The reaction mixture was stirred for 2.5 hours and monitored for consumption of 1-morpholino-2-(l-(trityloxy)but-3-en-2-yloxy)ethanone (target >97percent). The reaction mixture was quenched by charging into cold sat. aq. NH4CI (110 mL) and water (33 mL) while T < 20 ¡ãC. 2-Methoxy-2-methylpropane (218 mL) was added and the layers were separated. The organics were washed with sat. aq. NH4CI (65 mL) and 18percent aq. NaCl (44 mL.). The organics were concentrated under vacuum T < 25 ¡ãC to a light yellow oil of ketone 15 (21.6 g). According to the analysis of related databases, 38573-88-5, the application of this compound in the production field has become more and more popular. Reference:
Patent; ???????????????????????????; ? Buranko; Kimu ?; Chan ?; ?; Yoshizawa Kazuhiro; (94 pag.)JP2016/121177; (2016); A;,
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Application of 393-36-2, These common heterocyclic compound, 393-36-2, name is 4-Bromo-3-(trifluoromethyl)aniline, 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.

4-Bromo-3-(trifluoromethyl)aniline was converted into 4-bromo-3-(trifluoromethyl)phenyl isocyanate according to Method B1. According to Method C1a, 4-bromo-3-(trifluoromethyl)phenyl isocyanate was reacted with 4-(2-(N-methylcarbamoyl)-4-pyridyloxy)-2-chloroaniline to afford the urea. Entry 87: According to Method A2, Step 4, 4-amino-2-chlorophenol was reacted with 4-chloro-N-methyl-2-pyridinecarboxamide, which had been synthesised according to Method A2, Step 3b, to give 4-(2-(N-methylcarbamoyl)-4-pyridyloxy)-3-chloroaniline.

The synthetic route of 393-36-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER CORPORATION; US2003/144278; (2003); A1;,
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Reference of 33070-32-5, These common heterocyclic compound, 33070-32-5, name is 5-Bromo-2,2-difluorobenzodioxole, 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.

Preparation 67 2-(2,2-Difluorobenzo[d][1,3]dioxol-5-yl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane To a solution of 5-bromo-2,2-difluorobenzo[d][1,3]dioxole (1.5 g, 6.3 mmol) in N,N-dimethylformamide (12.7 mL) was added 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (1.6 g, 6.3 mmol), potassium acetate (1.9 g, 19.0 mmol), and (1,1′-bis(diphenylphosphino)ferrocene)-dichloropalladium(II) (0.3 g, 0.32 mmol). The reaction mixture was heated at 80 C. for 18 h, then the reaction mixture was diluted with Et2O and washed with water. The organic layers were separated, dried with Na2SO4, filtered, concentrated in vacuo, and purified by silica gel chromatography eluting with 0-100% acetone in hexanes to yield a brown oil (0.9 g, 50%): 1H NMR (400 MHz, DMSO-d6) delta 7.55 (d, J=8.0 Hz, 1H), 7.53 (s, 1H), 7.43 (d, J=8.0 Hz, 1H), 1.30 (s, 12H); 19F NMR (376 MHz, DMSO-d6) delta -49.26 (s); EIMS m/z 284.

The synthetic route of 33070-32-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dow AgroSciences LLC; Eckelbarger, Joseph D.; Epp, Jeffrey B.; Fischer, Lindsey G.; Lowe, Christian T.; Petkus, Jeff; Roth, Joshua; Satchivi, Norbert M.; Schmitzer, Paul R.; Siddall, Thomas L.; US2014/274701; (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. 22364-29-0, name is 2-Bromo-4,5-dimethylaniline, A new synthetic method of this compound is introduced below., COA of Formula: C8H10BrN

To a suspension of aniline ii (20.0 g, 100 mmol) in H2O (50 mL)was added 12 M HCl (100 mL) and the reaction mixture was cooled to 0 C, to which was gradually added NaNO2 (8.99 g, 130 mmol) in H2O (30 mL) followed by CuCl (12.1 g, 122 mmol) dissolved in 12 M HCl (30 mL) at same temperature. After warmed up to room temperature, the reaction was stirred for further 20 min. The products were extracted with Et2O (X3), and the combined organic extracts were washed with 25% NH3 aq. and brine, dried (Na2SO4), and concentrated in vacuo. Purification of the crude products by recrystallization from MeOH gave 1-bromo-2-chloro-4,5-dimethylbenzene (iii) (15.2 g, 69.2%) as colorless prisms.

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:
Article; Eda, Shohei; Hamura, Toshiyuki; Molecules; vol. 20; 10; (2015); p. 19449 – 19462;,
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Reference of 129316-09-2,Some common heterocyclic compound, 129316-09-2, name is 1,3-Dibromo-5-(tert-butyl)benzene, molecular formula is C10H12Br2, 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.

Step 1 : tert-Butyl 3-bromo-5-(tert-butvnbenzoate (P11a)n-BuLi (7.2 mL, 18.0 mmol, 2.5M in THF) was added to a flask under N2 containing toluene (9 mL) at -10C. >BuMgCI (4.5 mL, 9.0 mmol, 2M in THF) was then added at such a rate to keep the temperature below -5C. The resulting milky slurry was aged at -10C for 30 min, then 1 ,3- dibromo-5-(terf-butyl)benzene (6.2 g, 21.2 mmol) dissolved in toluene (20 mL) was added. The rate of addition was such that the temperature did not increase above -5C. After addition was complete, the mixture was kept at -10C until the metal-halogen reaction was complete. A solution of di-tert-butyl dicarbonate (5.89 g, 27 mmol) in toluene (7.5 mL) was then charged such at a rate to keep the temperature below -5C. After the addition was complete, the mixture was kept at -10C until the aryl-Mg intermediate was completely consumed. The mixture was quenched by the addition of 10% aq. citric acid (40 mL). The phases were separated and the organic layer was washed with another 10% aq. citric acid (40 mL). The organic extracts were dried over MgS04 and concentrated. Compound P11a (4.0 g, 60%) was obtained as a brown oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Dibromo-5-(tert-butyl)benzene, its application will become more common.

Reference:
Patent; PHENEX PHARMACEUTICALS AG; STEENECK, Christoph; KINZEL, Olaf; GEGE, Christian; KLEYMANN, Gerald; HOFFMANN, Thomas; WO2012/139775; (2012); A1;,
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These common heterocyclic compound, 4263-52-9, name is Sodium 2-bromoethanesulphonate, 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. Quality Control of Sodium 2-bromoethanesulphonate

b) Compound lb; [0169] A mixture of compound la, (0.1 g, 0.45 mmole), sodium 2- bromoethanesulfonate (0.19 g, 2 equivalents) and 2,6-di-tert-butylpyridine (99 muL, 0.45 mmole) in [BMIM]BF4] (1 mL, Aldrich) was heated in an oil bath at 150C with vigorous stirring for 16 hours. The reaction was then cooled to room temperature and a small portion of the reaction mixture was withdrawn, diluted with methanol/water and analyzed by analytical HPLC using a Phenomenex, Ci8,4.6 x 250 mm column and a 30 minute gradient of 10? 70% MeCN/water (with 0.05% TFA) at a flow rate of 1.0 mL/minute and UV detection at 260nm and 220 nm. Product was observed eluting at Rt = 13.3 minutes (-40% conversion). The reaction mixture was prepared by diluting it with water (15 mL) and washing this solution with ethyl acetate (2 x 25 mL). The aqueous solution was then treated with 3 to 4 drops of ammonia and further extracted with ethyl acetate (2 x 25 mL). The aqueous solution was then concentrated to about 7 mL by rotary evaporation. The product was then purified by preparative HPLC using an YMC, Ci8, 30 x 250 mm column and the same gradient as described above at a flow rate of 20 mL/minute. HPLC fractions containing product were combined and concentrated under reduced pressure. Yield = 30 mg (20%, white solid); MALDI-TOF MS 330.6 observed.

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

Reference:
Patent; SIEMENS HEALTHCARE DIAGNOSTICS INC.; NATRAJAN, Anand; SHARPE, David; WEN, David; JIANG, Qingping; WO2011/146595; (2011); A2;,
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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. 1422-53-3, name is 2-Bromo-4-fluorotoluene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: 2-Bromo-4-fluorotoluene

To a solution of 2-bromo-4-fluorotoluene (16.0 g) in anhydrous tetrahydrofuran was added dropwise at -78 C. a solution of 1.6M butyllithium in hexane (55.5 ml), and the mixture was stirred at the same temperature for 30 minutes. To the mixture was added dropwise a solution of dimethylformamide (6.8 g) in tetrahydrofuran (20 ml), and the mixture was allowed to stand to warm up to 0 C. To the reaction solution was added ice-water, and the reaction solution was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated to give oil of 5-fluoro-2-methylbenzaldehyde (11.5 g). To a mixture of acetone (80 ml), sodium hydroxide (3.7 g) and water (100 ml) was added dropwise at room temperature a solution of 5-fluoro-2-methylbenzaldehyde (11.5 g) in acetone (30 ml), and the mixture was stirred at the same temperature for 1 hour. Under reduced pressure, acetone was evaporated, and the residue was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and concentrated under reduced pressure to give 4-(5-fluoro-2-methylphenyl)-3-buten-2-one (13.4 g). To a solution of 20% sodium ethoxide in ethanol (5.9 g) was added at room temperature diethyl malonate (14.0 g), and then added little by little 4-(5-fluoro-2-methylphenyl)-3-buten-2-one (13.4 g), and the mixture was stirred at room temperature for 30 minutes and then for 2 hours while heating, and cooled. The solvent was evaporated, and to the residue was added water. The aqueous layer was washed with ethyl acetate and concentrated. To the residue was added 2M sodium hydroxide (46 ml), and the mixture was refluxed for 2 hours and cooled. To the mixture was added 2.5M sulfuric acid (46 ml) for 10 minutes, and the mixture was refluxed for 30 minutes and cooled. Precipitated crystals were filtered and washed with water and isopropylether to give 5-(5-fluoro-2-methylphenyl)cyclohexane-1,3-dione (8.6 g) as colorless crystals. mp 175-176 C. 1H-NMR(CDCl3) delta: 2.30 (3H, s), 2.27-2.56 (4H, m), 2.5-4.3 (1H, br), 3.44-3.63 (1H, m), 5.55 (1H, s), 6.77-7.01 (2H, m), 7.09-7.17 (1H, m).

The synthetic route of 1422-53-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Takeda Chemical Industries, Ltd.; US6350749; (2002); B1;,
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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. 553-94-6, name is 2,5-Dimethylbromobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C8H9Br

General procedure: In the reaction tube with a magnetic bar was added the solution of aryl bromides (0.5 mmol) and phenylboronic acid (91 mg, 0.75 mmol), NaOH (24 mg, 0.6 mmol), complex 1 (0.0001-0.02 mol%, dissolved in DMA) and ethanol (3 mL). After stirred for the required time in the preset conditions, the reaction mixture was cooled to room temperature, and then quenched by 1 mL brine and 3 mL water, and extracted with ethyl acetate (3¡Á5 mL). The combined organic layer was dried over anhydrous MgSO4 and the filtrate was concentrated to dryness under reduced pressure. The crude products were purified by column chromatography (petroleum ether, ethyl acetate) on silica gel.

The synthetic route of 553-94-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wu, Qinxu; Wu, Leilei; Zhang, Lei; Fu, Haiyan; Zheng, Xueli; Chen, Hua; Li, Ruixiang; Tetrahedron; vol. 70; 21; (2014); p. 3471 – 3477;,
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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. 33884-43-4, name is 2-(2-Bromoethyl)-1,3-dioxane, A new synthetic method of this compound is introduced below., SDS of cas: 33884-43-4

Sodium hydroxide (3.46g, 1.3 eq) was taken up in water (2OmL) and stirred for about 30 minutes. Then 3-tert-butyl phenol (10.0 g, 66.6 mmol) was added and the resulting mixture was stirred at room temperature for 30 minutes. Next, 2-(2-bromoethyl)-[l,3] dioxane (9.9 mL, 1.1 eq) was added ant the resulting mixture was heated at reflux for 40 hours. The reaction mixture was cooled to room temperature and then added ethyl acetate (150 mL) and with stirring acetic acid was added to pH = 4, followed by dilution with water (100 mL) and ethyl acetate (150 mL). After partitioning, the layers were separated and then washed the organic layer with water (3X 10OmL) and the ethyl acetate layers were dried over magnesium sulfate, filtered and concentrated to give the title compound as a colorless oil (16.9Ig).

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; F. HOFFMANN-LA ROCHE AG; DEWDNEY, Nolan James; HAWLEY, Ronald Charles; KONDRU, Rama K.; LAI, Yingjie; LOU, Yan; WO2010/122038; (2010); 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. 64695-79-0, name is 2-Bromo-4,5-difluoroaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 2-Bromo-4,5-difluoroaniline

To a mixture of compound 47a (10 g, 48.08 mmol) and compound 47b (20.84 g, 57.69 mmol) in toluene (200 mL) was added Pd (PPh3) 4 (2.78 g, 2.4 mmol) in one portion under N 2. The resulting black mixture was stirred at 100C for 12 h under N 2. The reaction was cooled to 25C and then treated with 6N HCl (10 mL) with stirring at 25C for 1h. It was diluted with water (400 mL) and extracted with EtOAc (120 mL 3). The combined organic layers was washed with 20%KF solution (200 mL) and brine (100 mL) successively, dried over sodium sulfate and concentrated in vacuum to give the crude product, which was purified by column chromatography on silica gel (5%EtOAc in petroleum ether) to give compound 47c (4.2 g, 51% yield) as a yellow solid. LCMS: R t = 0.709 min in 5-95AB_220&254. lcm chromatography (MERCK RP18 2.5-2mm), MS (ESI) m/z=171.9 [M+H] +. 1H NMR: (400MHz, CDCl 3) delta 7.50 (dd, J=8.8 Hz, 11.2 Hz, 1H), 6.41 (dd, J=6.8 Hz, 12.0 Hz, 1H), 6.37-6.17 (m, 2H), 2.52 (s, 3H).

The synthetic route of 64695-79-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DIZAL (JIANGSU) PHARMACEUTICAL CO., LTD; LI, Zhengtao; ZOU, Hao; ZHU, Wei; SHEN, Changmao; WANG, Rumin; LIU, Wengeng; CHEN, Xiang; TSUI, Honchung; YANG, Zhenfan; ZHANG, Xiaolin; (307 pag.)WO2019/149164; (2019); A1;,
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