Category: bromides-buliding-blocks

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. 69038-76-2, name is 4-Bromo-N1-methylbenzene-1,2-diamine, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 4-Bromo-N1-methylbenzene-1,2-diamine

Ste 3. 5-Bromo-l-methyl-7H-benzo[Patent; BIOENERGENIX; MCCALL, John M.; ROMERO, Donna L.; KELLY, Robert C.; WO2012/119046; (2012); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 558-13-4, name is Carbontetrabromide, A new synthetic method of this compound is introduced below., Application In Synthesis of Carbontetrabromide

b 3-(Fluoro)phenethyl bromide To a solution of 3-(fluoro)phenethyl alcohol (3.8 g, 27.0 mmol), in anhydrous dichloromethane (100 ml), cooled to 0 C., was added carbon tetrabromide (11.25 g, 34.0 mmol) and triphenylphosphine (10.62 g, 41.0 mmol). After stirring for 0.5 h the solvent was removed in vacuo and diethyl ether (100 ml) was added to the residue. The resultant precipitate was removed by filtration, the filtrate evaporated under reduced pressure and the crude product chromatographed on silica-gel eluding with ethyl acetate/hexane (1:1) to give 3-(fluoro)phenethyl bromide (5.51 g, 100%), delta (250 MHz, CDCl3) 3.16 (2H, t, J=7.4 Hz, CH2), 3.57 (2H, t, J=7.4 Hz, CH2), 6.91-7.01 (3H, m, Ar–H), 7.24-7.33 (1H, m, Ar–H).

The synthetic route of 558-13-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merck Sharp & Dohme, Ltd.; US5889008; (1999); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 51437-00-4, name is 4-Bromo-1-fluoro-2-methylbenzene, belongs to bromides-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 51437-00-4, category: bromides-buliding-blocks

Under N2 atmosphere, an oven-dried 4 mL vial was charged with 2-fluoro-5- bromotoluene (56.7 mg, 38.3 mu, 0.300 mmol, 1.00 equiv), palladium complex 1 (11.4 mg, 15.0 muetaiotaomicron, 5.00 mol ), Ag(bipy)2C104 (16.0 mg, 30.0 muetaiotaomicron, 10.0 mol ), and NFBS (0.189 g, 0.600 mmol, 2.00 equiv). Acetonitrile (0.75 mL, c = 0.40 M) was added and the reaction mixture was stirred in a sealed vial at 23 C for 24 h. Subsequently, triethylamine (30.5 mg, 42.0 mu, 0.300 mmol, 1.00 equiv) was added and the reaction mixture was concentrated in vacuo. The residue was purified by chromatography on silica gel, eluting with hexanes/EtOAc (19: 1 to 4: 1 with 1% triethylamine), to afford 71.0 mg of the mixture of the title compounds as a yellow solid (63% yield). [00232] The products could not readily be separated by silica gel chromatography or preparative TLC, so they were characterized as a mixture. Compounds 2p-2p-IV were assigned through a combination of 1-D TOCSY and NOESY experiments (see page S92- S93). Data for 2p and 2p-II and 2p-III: [00233] R/= 0.57 (hexanes/EtOAc 7:3 (v/v)). NMR Spectroscopy: 1H NMR (600 MHz, CDC13, 23 C, delta): 8.07 (d, J = 8.2 Hz, 1.3H), 8.00 (d, J = 8.2 Hz, 4H), 7.96 (d, J = 8.2 Hz, 0.4H), 7.91 (d, J = 8.2 Hz, 0.6H), 7.72-7.68 (m, 2.9H), 7.66-7.62 (m, 0.3H), 7.59-7.54 (m, 5.7H), 7.53-7.49 (m, 0.7H), 7.46-7.42 (m, 1.5H), 7.31-7.27 (m, 0.2H), 7.25-7.22 (m, 0.2H), 7.01 (dd, J = 8.7, 8.7 Hz, 0.45H), 6.87 (dd, J = 9.6, 9.6 Hz, 0.2H), 6.81 (d, J = 9.6 Hz, 1H), 5.01 (s, 0.3H), 2.30 (s, 3H), 2.21 (s, 0.2H), 1.84 (s, 1.0H). 13C NMR (125 MHz, CDC13, 23 C, delta): Peaks are not listed because the mixture of four compounds, as well as splitting of aryl carbons by 19F, precluded assignment. See S91 for spectrum. Mass Spectrometry: HRMS (ESI-TOF) (m/z): calcd for Ci9H15BrNNa04S2 ([M + Na]+), 505.9504, found, 505.9502.

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:
Patent; PRESIDENT AND FELLOWS OF HARVARD COLLEGE; NGAI, Ming-Yu; BOURSALIAN, Gregory, Bagrad; MCNEILL, Eric, Andrew; RITTER, Tobias; WO2015/31725; (2015); A1;,
Bromide – Wikipedia,
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Some common heterocyclic compound, 827-08-7, name is 1,2-Dibromo-3,4,5,6-tetrafluorobenzene, molecular formula is C6Br2F4, 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. Product Details of 827-08-7

Butyllithium (1.6 M in hexanes, 12.6 mL, 20.16 mmol) was added dropwise to a stirred solution of 1,2-dibromotetrafluorobenzene (2.6 g, 8.44 mmol) in ether (50 mL) at -78 C. After 2 hours this solution was slowly added to a pre-cooled solution (-78 C.) of trimethylborate (2.3 mL, 20.52 mmol) in ether (25 mL). The resulting suspension was stirred at -78 C. for two hours then gradually warmed to room temperature and hydrolyzed with 20 mL of 10% HCl. The yellow organic phase was separated and the aqueous phase was extracted with dichloromethane (3*15 mL). The combined organic phases were washed with water (3*10 mL) and dried over magnesium sulfate. Removal of solvent under reduced pressure gave a yellow oil that was recrystallized from water at a pH of 4 to afford a crystalline solid. (1.5 g, 75%) 19F NMR (D2O/HCl) delta: -136.6 (d, JF-F=28.3 Hz, 2F, C6F4), -156.5 (d, JF-F=28.3 Hz, 2F, C6F4). 11B NMR (D2O/HCl) delta: 16.9 (br).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 827-08-7, its application will become more common.

Reference:
Patent; Piers, Warren Edward; Chase, Preston A.; Henderson, Lee Douglas; US2005/222463; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 626-39-1, name is 1,3,5-Tribromobenzene, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 626-39-1

n-Butyllithium (2.5 mL of a 2.5 mol/l solution in n-hexane,6.3 mmol) was added to a solution of 1,3,5-tribromobenzene (7) (2.00 g, 6.35 mmol) in Et2O (40mL) at -78 C under inert atmosphere. After 10 min, CuCN (282 mg, 3.18 mmol) was added andthe reaction mixture was allowed to warm up to -60 C within 90 min. Nitrobenzene (0.98 mL,9.53 mmol) was then added in one portion and the dark solution stirred while warming toambient temperature (16 h). An aqueous solution of NH3 (12.5% w/w, 80 mL) was slowly addedand the resulting mixture was extracted with MTBE (3 x 50 mL). The combined organic layerswere washed with water (50 mL) and brine (50 mL), dried over MgSO4, filtered and the solventwas removed in vacuum. Further purification was accomplished by column chromatography(SiO2, n-hexane, Rf 0.69). The resulting material was washed with acetone (20 mL) to give theproduct 8 as a colorless solid (722 mg, 1.54 mmol, 48%), mp 190 C (ref.22 190-191 C). 1HNMR (500 MHz, CDCl3): delta 7.70 (t, J 1.7 Hz, 2 H), 7.59 (d, J 1.7 Hz, 4 H) ppm. 13C{1H} NMR(126 MHz, CDCl3): delta 141.8 (2 C), 133.9 (2 CH), 129.0 (4 CH), 123.6 (4 C) ppm. IR (ATR):3103 (w), 3068 (m), 1579 (m), 1541 (s), 1407 (m), 1387 (m), 1098 (m), 1068 (m), 847 (s), 752(s), 672 (m), 653 (m) cm-1. MS (EI, 70 eV), m/z (%): 466 (95) [M+], 308 (25), 150 (25), 84(100). Anal. calcd. for C12H6Br4 (469.80): C 30.68, H 1.29; found C 30.68, H 1.30.

According to the analysis of related databases, 626-39-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Behler, Florian; Wickleder, Mathias S.; Christoffers, Jens; ARKIVOC; vol. 2015; 2; (2014); p. 64 – 75;,
Bromide – Wikipedia,
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Synthetic Route of 3972-64-3, These common heterocyclic compound, 3972-64-3, name is 1-Bromo-3-(tert-butyl)benzene, 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 36: 3-t-butyl benzaldehyde3-t-butyl phenylbromide was dissolved in THF and n-BuLi was added thereto, followed by addition of DMF and stirring at 0¡ãC for 3 hours. After the reaction was complete, NH4Cl was added to the reaction mixture, followed by extraction with EtOAc. The organic extract was dried over MgSO4 and concentrated under reduced pressure. The residue was purified by column chromatography (eluent: EtOAc: n-Hex = 1/3) to afford the title compound (339 mg, 80percent).MS|M+1] = 163 (M+1)

The synthetic route of 3972-64-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LG LIFE SCIENCES, LTD.; WO2009/38412; (2009); A2;,
Bromide – Wikipedia,
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Synthetic Route of 1647-26-3, 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. 1647-26-3, name is 1-Bromo-2-cyclohexylethane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

[00319] A reaction vial was charged with N-(quinolin-3-yl)-5,6,7,8-tetrahydro-2,6-naphthyridin-1-amine (15.00 mg, 0.05428 mmol), 2-bromo ethylcyclohexane (10.4 mg, 0.0000543 mol), NN- diisopropylethylamine (0.0189 mL, 0.000108 mol) and acetonitrile (1 mL, 0.02 mol) and the reaction heated in a microwave at 120 0C for 1 h. The reaction was then quenched with water and extracted with dichloromethane. The solvent was removed and the residue purified by prep HPLC to get the product as peach colored solid. MS (M+H)= 386.9;1H-NMR (DMSOd6I3): (400 MHz) 59.09 (d, J=2.12Hz, IH), 8.70 (d, J=I .87 Hz, IH), 8.26 (s, IH), 7.98 (d, J=5.34 Hz, IH), 7.90 (d, J=8.85 Hz, IH), 7.83 (d, J=7.58 Hz, IH), 7.56-7.48 (m, 2H), 6.64 (d, 7=5.38 Hz, IH), 3.49 (s, 2H), 2.74 (s, 4H), 1.80-0.85 (m, 15 H)

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-Bromo-2-cyclohexylethane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; RENOVIS, INC.; WO2009/11904; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 586-61-8, name is 1-Bromo-4-isopropylbenzene, belongs to bromides-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 586-61-8, name: 1-Bromo-4-isopropylbenzene

1.07 g of 0.01 mol of 3-methylaniline, 1.98 g of 0.01 mol of 4-bromoisopropylbenzene, and 3.1 g of sodium t-butoxide were added to a 100 ml three-necked flask, dissolved in 30 ml of toluene solution, and then 0.1 g of pd2 was added under nitrogen atmosphere. (dba) 3, 0.67 g of 10% tri-tert-butylphosphine, heating at 10 C, stirring for 3 hours, the reaction is complete, adding 25 ml of toluene, 25 ml of water, liquid separation, adding the organic phase column to silica gel spin-drying, column chromatography (solvent Ethyl acetate / petroleum ether = 1:20),The column was spun dry to give 1.7 g of white intermediate A2-1, yield 76%.

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-Bromo-4-isopropylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Beijing Dingcai Technology Co., Ltd.; Gu’an Dingcai Technology Co., Ltd.; Fan Hongtao; Tian Lei; Ren Xueyan; Zhang Xianghui; (35 pag.)CN108129431; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 452-74-4, name is 1-Bromo-2-fluoro-4-methylbenzene, molecular formula is C7H6BrF, 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 1-Bromo-2-fluoro-4-methylbenzene

1-Bromo-4-(bromomethyl)-2-fluorobenzene: In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a solution of commercially available 1-bromo-2-fluoro-4-methylbenzene (1.37 mL, 106 mmol) in AcCN (25 mL) was treated with /V-bromosuccinimide (2.83 g, 15.9 mmol) and the reaction mixture was heated to 80 C before to add benzoyl peroxide (2.73 mg, 8.46 mmol) and the reaction mixture was stirred for 1.5 h at 80 C. The reaction mixture was partitioned between water (30 mL) and EA (20 mL). The org. layer was washed with brine, dried over MgS04, filtered, and the solvent was removed under reduced pressure. Purification of the residue by FC (1 : 19? 1 : 10 EA/hept) gave the title compound as yellow oil: TLC: rf (1 :10 EA/hept) = 0.58. LC-MS-conditions 07: tR = 0.91 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 452-74-4, its application will become more common.

Reference:
Patent; ACTELION PHARMACEUTICALS LTD; CORMINBOEUF, Olivier; CREN, Sylvaine; LEROY, Xavier; POZZI, Davide; WO2015/19325; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 583-75-5, 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. 583-75-5 name is 4-Bromo-2-methylaniline, 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.

Step A: ammonium tetrafluoroborate (20.97 g, 200 mmol) was dissolved in aqueous acetic acid (500 ML AcOH/250 ML water) and cooled to 0 C. 2-Methyl-4-bromoaniline (18.61 g, 100 mmol) and 42 ML of aqueous concentrated HCl (36% w/w, 12N, 500 mmol) were sequentially added.The mixture was stirred for 20 minutes at 0 C. and NaNO2 (7.59 g, 110 mmol) was added.The reaction was stirred for 1 hour at 0 C. and warmed to room temperature.After 16 hours at room temperature, the mixture was concentrated under reduced pressure and the residue was azeotroped with toluene and dried under high vacuum.The solid was suspended in 500 ML of CHCl3 and KOAc (12.76 g, 130 mmol) and 18-crown-6 (7.93 g, 30 mmol) were added.The reaction was stirred for 1.5 hours at room temperature.The mixture was washed with water, dried over anhydrous MgSO4, filtered through Celite and concentrated under reduced pressure to provide 30 g of 5-bromo-1H-indazole (compound 2f) as a tan solid.The crude material was used without further purification.

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

Reference:
Patent; Munson, Mark; Rizzi, James; Rodriguez, Martha; Kim, Ganghyeok; US2004/176325; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary