Author: Jessica.F

Adding a certain compound to certain chemical reactions, such as: 24358-62-1, name is 1-(4-Bromophenyl)ethylamine, 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 24358-62-1, category: bromides-buliding-blocks

l-(4-Bromophenyl)ethanamine (3.58 ml, 25 mmol) and Et3N (4.39 ml, 31.25 mmol) was dissolved in CH2Cl2 and cooled to 00C. To this was added (Boc)2O (6.0 g, 27.5 mmol) and the resulting solution was stirred 5 minutes at 00C for 5 and then 3 h at room temperature. The reaction was washed with HCl (50 ml, IM) followed by NaHCO3 (sat) (2*50 ml). The organic phase was dried over MgSO4, filtered and evaporated. The residue was purified by precipitation from MeOH/H2O (10:1) to give 6.35 g (85%) of the title compound as a white powder.1H NMR (CDCl3) delta 7.45 (d, 2H), 7.18 (d, 2H), 4.83-4.70 (br, 2H), 1.46-1.32 (br, 12H).

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; RESPIRATORIUS AB; JOHANSSON, Martin; THORNQVIST-OLTNER, Viveca; TOFTERED, Joergen; WENSBO, David; DALENCE, Maria; WO2010/97410; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 39478-78-9, 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. 39478-78-9, name is 5-Bromo-2-methylaniline, This compound has unique chemical properties. The synthetic route is as follows.

A solution of sodium nitrite (4.08 g, 53.7 mmol, 1.10 equiv) in water (40 mL) was added slowly to a pre-cooled (-10 C) mixture of finely powdered 5-bromo-2-methylaniline (6-1, 10.0 g, 54.5 mmol, 1 equiv) and concentrated aqueous hydrochloric acid solution (12 M, 13.4 mL, 161 mmol, 3.00 equiv) in water (70 mL) at a rate that kept the reaction mixture temperature below 0 C. Following the addition, the reaction mixture was stirred at -5 C for 30 min, then filtered. A solution of sodium tetrafluoroborate (17.7 g, 161 mmol, 3.00 equiv) in water (50 mL) was immediately added to the cold filtrate. The precipitate was filtered and washed with ice-cold water (30 mL). The remaining solid was air-dried to give 5-bromo-2-methylbenzenediazonium tetrafluoroborate as a white solid. A suspension of this product (15.0 g, 52.7 mmol, 1 equiv), potassium acetate (12.9 g, 132 mmol, 2.50 equiv) and 18- crown-6 (1.39 g, 5.27 mmol, 0.100 equiv) in chloroform (300 mL) was stirred at 23 C for 20 h. The reaction mixture was filtered and concentrated. The residue was partitioned between water and EtOAc (500 mL). The organic layer was washed with brine, dried over sodium sulfate and concentrated to give 6-bromo-1H-indazole (6-2) as a tan solid. 1H NMR (300 MHz, CDCl3) delta 10.20 (br s, 1H), 8.06 (br s, 1H), 7.70 (s, 1H), 7.63 (d, 1H, J = 8.5 Hz), 7.29 (dd, 1H, J = 8.5, 1.5 Hz).

The chemical industry reduces the impact on the environment during synthesis 5-Bromo-2-methylaniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; MERCK & CO., INC.; WO2006/86255; (2006); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 18648-66-3, 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. 18648-66-3, name is 2-(4-Bromophenyl)-1,1-diphenylethylene, This compound has unique chemical properties. The synthetic route is as follows.

Into a 500 ml three-necked flask equipped with a condenser, 0.16 g (6.6 mmole) of magnesium, a small piece of iodine and 10 ml of THF were placed under a stream of argon. After the resultant mixture was stirred at the room temperature for 30 minutes, a solution prepared by dissolving 1 g (3 mmole) of 1-(4-bromophenyl)-2,2-diphenylethylene into 10 ml of THF was added dropwise. After the addition was completed, the resultant mixture was stirred at 60C for 1 hours, and a Grignard reagent was prepared. Into a 500 ml three-necked flask equipped with a condenser, 0.45 g (1 mmole) of 2,6/2,7-di-t-butyl-9,10-dibromoanthracene, 0.04 g (5% by mole) of dichlorobis(triphenylphosphine)palladium, 0.1 ml (1M; 0.1 mmole) of a toluene solution of diisobutylaluminum hydride and 10 ml of THF were placed under a stream of argon. After the Grignard reagent prepared above was added dropwise to the obtained solution at the room temperature, the resultant mixture was heated under stirring for one night. After the reaction was completed, the reaction solution was cooled with ice water. The formed crystals were separated by filtration and washed with 50 ml of methanol and 50 ml of acetone successively, and 0.4 g of a yellow powder was obtained. The obtained yellow powder was identified to be Compound (A2) by the measurements in accordance with NMR, IR and FD-MS (the yield: 50%).

The chemical industry reduces the impact on the environment during synthesis 2-(4-Bromophenyl)-1,1-diphenylethylene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; EP1440959; (2004); A1;,
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. 4333-56-6, name is Bromocyclopropane, A new synthetic method of this compound is introduced below., Recommanded Product: Bromocyclopropane

To a degassed solution of potassium te/t-butoxide (2.08 g, 18.51 mmol) in dry di- methylsulphoxide (6 ml_), 4-bromo-benzenethiol (3.5 g, 18.5 mmol) was added and the mixture was stirred for 15 min at ambient temperature under nitrogen. Bromocyclopropane (4.4 ml_, 55.5 mmol) was added afterwards and the reaction mixture was heated at 80 C for 24 h in a sealed vessel. The mixture was cooled, diluted with ether (150 ml.) and washed with water (100 ml_). The aqueous layer was extracted with ether (3 x 50 ml_). Combined organic extracts were finally dried with anhydrous magnesium sulfate. i-Bromo-4-cyclopropyl- sulfanyl-benzene was obtained after evaporation of the solvent as yellow liquid. Yield: 3.49 g (82 %).RF (SiO2, hexanes/ethyl acetate 4:1 ): 0.70.1H NMR spectrum (300 MHz, CDCI3, deltaH): 7.40 (d, J=8.6 Hz, 2 H); 7.23 (d, J=8.5 Hz, 2 H); 2.16 (m, 1 H); 1.08 (m, 2 H); 0.69 (m, 2 H).

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; NOVO NORDISK A/S; WO2007/71766; (2007); 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. 454-79-5, name is 2-Bromo-5-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., name: 2-Bromo-5-(trifluoromethyl)aniline

Isonicotinoyl chloride hydrochloride (427 mg, 2.39 mmol, commercially available product) and triethylamine (410 mul, 2.94 mmol) were sequentially added at 0C to a dichloromethane (5 ml) solution of 2-bromo-5-(trifluoromethyl)aniline (480 mg, 2.00 mmol; commercially available product). The resulting mixture was warmed to room temperature and stirred for 24 hours. Water was added to the mixture, and the resulting mixture was extracted three times with ethyl acetate. The obtained organic layer was washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by recrystallization (ethyl acetate). Thus, N-[2-bromo-5-(trifluoromethyl)phenyl]isonicotinamide (GIF-0612) (308 mg, 44.8%) was yielded as a colorless solid. TLC Rf 0.46 (hexane/ethyl acetate = 1/1).

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; HAGIWARA, Masatoshi; EP1712242; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 40161-54-4, The chemical industry reduces the impact on the environment during synthesis 40161-54-4, name is 1-Bromo-2-fluoro-4-(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

To a mixture of l-bromo-2-fluoro-4-(trifluoromethyl)benzene (5.0 g, 0.02 mol) in EtOH (10 mL) was added Pd(dppf)Ci2 (1.46 g, 0.2 mmol ) and AcONa (3.37 g, 0.041 mol), and the resulting mixture was stirred at 80 C under an atmosphere of CO (50 psi) for 8 hours. The mixture was then filtrated and the filtrate was partitioned with ethyl acetate and water. The aqueous layer was separated and extracted with ethyl acetate twice. The combined organic layers were washed with brine, dried over anhydrous Na2S04 and concentrated in vacuo. The resulting residue was purified by column chromatography on silica gel (eluting with PE_EA=10: 1) to give the title compound. NMR (400MHz, CDC13) & 8.04-8.08 (t, 1H, J= 7.6 Hz), 7.49-7.47 (d, 1H, J = 8.0 Hz), 7.43-7.40 (d, 1H, J= 10.4 Hz), 4.44-4.40 (q, 2H, J= 7.2 Hz), 1.43-1.38 (t, 3H, J= 7.2 Hz).

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-fluoro-4-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK SHARP & DOHME CORP.; BIFTU, Tesfaye; COLLETTI, Steven L.; HAGMANN, William K.; KAR, Nam Fung; JOSIEN, Hubert; NAIR, Anilkumar; NARGUND, Ravi; BIJU, Purakkattle; ZHU, Cheng; HU, Bin; WO2015/51496; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 399-94-0, name is 1-Bromo-2,5-difluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C6H3BrF2

2-bromo-l,4-difluorobenzene (1.5 eq.) was dissolved in 4 volumes of THF (based on weight of tert-butyl2-oxopyrrolidine-l-carboxylate) and cooled to about 5 Celsius. A solution of 2.0 M iPrMgCl in THF (1.4 eq.) was added over 2 hours to the mixture while maintaining a reaction temperature below 25 Celsius. The solution was allowed to cool to about 5 Celsius and stirred for 1 hour (GC analysis confirmed Grignard formation). A solution of tert-butyl 2-oxopyrrolidine-l-carboxylate (1.0 eq.) in 1 volume of THF was added over about 30 min while maintaining a reaction temperature below 25 Celsius. The reaction was stirred at about 5Celsius for 90 min (tert-butyl 2-oxopyrrolidine-l-carboxylate was confirmed to be less than 0.5 area % by HPLC). The reaction was quenched with 5 volumes of 2M aqueous HC1 while maintaining a reaction temperature below 45 Celsius. The reaction was then transferred to a reparatory funnel adding 10 volumes of heptane and removing the aqueous layer. The organic layer was washed with 4 volumes of saturated aqueous NaCl followed by addition of 2×1 volume of saturated aqueous NaCl. The organic layer was solvent-switched to heptane (<1% wt THF confirmed by GC) at a distillation temperature of 35-55 Celsius and distillation pressure of 100-200 mm Hg for 2x4 volumes of heptane being added with a minimum distillation volume of about 7 volumes. The mixture wasthen diluted to 10 volumes with heptane while heating to about 55 Celsius yielded a denser solid with the mixture being allowed to cool to room temperature overnight. The slurry was cooled to less than 5 Celsius and filtered through polypropylene filter cloth. The wet cake was washed with 2x2 volumes of heptane. The solids were dried under vacuum at 55 Celsius until the weight was constant, yielding tert-butyl (4-(2,5-difluorophe-nyl)-4-oxobutyl)-carbamate as a white solid at about 75% to 85% theoretical yield. The synthetic route of 399-94-0 has been constantly updated, and we look forward to future research findings. Reference:
Patent; Array BioPharma, Inc.; Arrigo, Alisha B.; Juengst, Derrick; Shah, Khalid; (70 pag.)US2016/137654; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 40161-54-4, name is 1-Bromo-2-fluoro-4-(trifluoromethyl)benzene, 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 40161-54-4, HPLC of Formula: C7H3BrF4

Intermediate H: l-(2-Bromo-5-(trifluoromethyl)phenyl)-lH-imidazole A microwave vial charged with a solution of potassium tert-butoxide (0.462 g, 4.12 mmol), imidazole (0.280 g, 4.12 mmol), and l-bromo-2-fluoro-4- (trifluoromethyl)benzene (1.000 g, 4.12 mmol) in 2mL DMF was heated to 150 C in an oil bath overnight. The reaction mixture was diluted with DCM, filtered through a syringe filter, and concentrated. Purification of the resulting residue by silica gel column chromatography (0 to 100% EtOAc/heptane) gave l-(2-bromo-5- (trifluorom 291.0

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; AMGEN INC.; DINEEN, Thomas; KREIMAN, Charles; WEISS, Matthew; GEUNS-MEYER, Stephanie; WO2013/134518; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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 3638-73-1 as follows. Safety of 2,5-Dibromoaniline

2, 5-Dibromoaniline was recrystallized from a mixture of toluene/hexane solvents. Under nitrogen, 2, 6-dibromoaniline (36.1 g, 144.0 mmol) and quinoline-6-carbonyl chloride (Precursor 1, 27.3 g, 142.0 mmol, 0.99 equivalent) were dissolved in anhydrous 1, 4-dioxane (350.0 mL) in a 1L one-neck RBF equipped with a large stirrer bar and a reflux condenser. While stirring the solution, a Huenig base (37.2 g, 288.0 mmol, 2.0 equivalents) was added to the solution. The contents in the flask were heated to about 40 by an exothermic reaction. The mixture was stirred and cooled to room temperature. The reactants were heated to 100 in an oil bath for 20 hrs. A complete consumption of 2, 5-dibromoaniline was monitored by TLC. The reactants were poured into warm water (1.5 L) and fine deposits were then formed. The solution was neutralized with sodium carbonate and filtered. The collected residue was dried by suction and rinsed with acetone (25.0 mL) and toluene (25.0 mL) . The filter cake was transported to a 1 L flask, trace water was removed by azeotropic distillation with toluene on a rotary evaporator, and the cake was kept under high-degree vacuum overnight. The dried residue was recrystallized from monochlorobenzene (1.5 L) by using activated carbon as a decolorant. The crystals were separated by filtration and dried under high-degree vacuum (45.05 g, 111.0 mmol, 77.1 , off-white needles) . Addition purification was effected by recrystallization from 1, 4-dioxane ( 0.9 L) . The final product was obtained in the form of off-white crystal (plate) (40.0 g, 98.5 mmol, 68.5) . [0102] 1H NMR (500 MHz, DMSO-d6) delta 10.38 (s, 1H) , 9.03 (dd, J 4.2, 1.7 Hz, 1H) , 8.68 (d, J 2.0 Hz, 1H) , 8.55 (ddd, J 8.3, 1.6, 0.8 Hz, 1H) , 8.28 (dd, J 8.8, 2.0 Hz, 1H) , 8.16 (d, J 8.8 Hz, 1H) , 7.87 (d, J 2.4 Hz, 1 H) , 7.71 (d, J 8.6 Hz, 1 H) , 7.65 (dd, J 8.3, 4.2 Hz, 1H) , 7.46 (dd, J 8.6, 2.4 Hz, 1 H) 13C-NMR (126 MHz, DMSO-d6) delta 119.73, 120.70, 122.78, 127.59, 128.26, 129.19, 129.77, 131.01, 131.25, 132.09, 134.78, 137.63, 138.58, 149.45, 152.86, 165.52. GC/CI+ m/z () : 404.96 (50) [M+H, 2 × 79Br] +, 406.97 (100) [M+H, 79Br, 81Br] +, 408.96 (50) [M+H, 2 × 81Br] +.

According to the analysis of related databases, 3638-73-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; DOW GLOBAL TECHNOLOGIES LLC; ROHM AND HAAS ELECTRONIC MATERIALS KOREA LTD.; CHO, Sang Hee; NA, Hong Yeop; TANG, Zhengming; FENG, Shaoguang; MOON, Doo-Hyeon; (43 pag.)WO2017/156698; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 955959-84-9, A common heterocyclic compound, 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, molecular formula is C18H11BrO, 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.

A mixture of 3.6 g (4.3 mmol) N4,N4?-di(biphenyl-4-yl)-N4-(10,10-dimethyl-10H-indeno[2,1-b]triphenylen-12-yl)biphenyl-4,4?-diamine, 1.6 g (5.0 mmol) of 4-(4-bromophenyl)dibenzo[b,d]furan, 0.025 g (0.1 mmol) of palladium(II)acetate, 0.07 g (0.19 mmol) of 2-(dicyclohexylphosphino)biphenyl, 0.65 g (7 mmol) of sodium tert-butoxide and 50 ml of toluene was refluxed under nitrogen overnight. After finishing the reaction, then cooled to room temperature. The organic layer was extracted with dichloromethane and water, dried with anhydrous magnesium sulfate, the solvent was removed and the residue was purified by column chromatography on silica gel (hexane-dichloromethane) to give product 2.8 g (yield 61percent) as a yellow solid. MS (m/z, FAB+):1072.1

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; YEN, FENG-WEN; (36 pag.)US2016/343941; (2016); A1;,
Bromide – Wikipedia,
bromide – Wiktionary