Month: May 2021

Related Products of 7314-86-5, 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. 7314-86-5, name is 1,3,5,7-Tetrabromoadamantane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1,3-dibromobenzene (70 mL) was added to a mixture of 1,3,5,7-tetrabromoadamantane (5.0 g, 11.1 mmol) and AlCl3 powder (4.0 g,30.0 mmol), at 0 C. The mixture was then stirred at ambient temperaturefor 36 h. After quenching the reaction by adding ice water, theorganic layer was diluted with chloroform and filtered. The filtrate waswashed with deionised water and brine and then dried over magnesiumsulfate. After evaporation to remove volatiles, 1,3,5,7-tetrakis(1,3-bibromophenyl)adamantane was obtained as a white solid from thecrystallization in chloroform (9.6 g, 81% yield). 1H NMR (DMSO-d6,400 MHz): delta (ppm) 7.80 (s, 8H), 7.69 (s, 4H), 2.05 (s, 12H); 13C NMR(CDCl3-d3, 400 MHz): delta (ppm) 150.7, 131.5, 126.2, 122.4, 45.3, 38.3.Anal. Calcd for C34H24Br8: C, 38.10; H, 2.26; Found: C, 38.11; H, 2.21.

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, 1,3,5,7-Tetrabromoadamantane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Li, Xiong; Guo, Jianwei; Tong, Rui; Topham, Paul D.; Wang, Jiawei; Reactive and functional polymers; vol. 130; (2018); p. 126 – 132;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 1150102-47-8, 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. 1150102-47-8, name is 6-Bromo-N1-methylbenzene-1,2-diamine belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a mixture of 3-bromo-N2-methyl-benzene-1,2-diamine (20.0 g, 99.4 mmol) in ACN (300 mL) was added CDI (32.2 g, 198 mmol). The reaction mixture was stirred at 85 C. for 12 hours under N2 atmosphere. On completion, the reaction mixture was concentrated in vacuo. The reaction mixture was diluted with water (200 mL), where a solid precipitate was formed, which was filtered off. The solid was washed with water (1 L) and dried in vacuo to give the title compound (20.0 g, 88% yield) as white solid. 1H NMR (400 MHz, DMSO-d6) delta 11.17 (s, 1H), 7.14 (dd, J=1.2, 8.0 Hz, 1H), 7.00-6.95 (m, 1H), 6.93-6.87 (m, 1H), 3.55 (s, 3H).

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, 6-Bromo-N1-methylbenzene-1,2-diamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Kymera Therapeutics, Inc.; Mainolfi, Nello; Ji, Nan; Kluge, Arthur F.; Weiss, Matthew M.; Zhang, Yi; (1443 pag.)US2019/192668; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 103275-21-4, 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. 103275-21-4, name is 3-Bromo-4-(tert-butyl)aniline, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 3-bromo-4- tert-butyl-phenylamine (5.00 g, 21.92 mmol) in 80 mL of DCM and 25 mL of methanol was added calcium carbonate (4.39 g, 43.83 mmol), followed by iodinating reagent (8.55 g, 21.92 mmol). The reaction was stirred for 3 h at room temperature, quenched with water 100 mL, and the product extracted into ethyl acetate (100 mL). The organic layer was washed with brine (75 mL), dried over magnesium sulfate and concentrated. Silica gel chromatography eluting with 25% ethyl acetate/hexane gave the product as an oil (4.50 g, 12.7 mmol, 58%) : 1H NMR (400 MHz, CDC13) 6 7. 61 (s, 1 H), 6.99 (t, J = 0.9 Hz, 1H), 3 : 96 (s, 2H), 1.44 (s, 9H); MS (ESI) 356.3.

The chemical industry reduces the impact on the environment during synthesis 3-Bromo-4-(tert-butyl)aniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; WO2005/70407; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 627526-90-3, 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. 627526-90-3, name is 1-Bromo-3-(difluoromethyl)-5-fluorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

steps 3-5; – /?-Methoxybenzyl alcohol (36.8 g, 266.7 mmol) was added slowly to a mixture of potassium t-butoxide (28.7 g, 255.5 mol) and THF (250 mL). After stirring for about 15 min, 30 (50.O g, 222.2 mmol) was added and the reaction mixture heated to about 65 C. After stirring at 65 C for 2 h, the reaction is analyzed by HPLC. After cooling to RT, a mixture of saturated NaHCO3 solution (150 mL) and water (150 mL) was added. Toluene (300 mL) was added, the organic phase separated and washed with a mixture of saturated NaHCO3 solution (75 mL) and water (75 mL). Polish filtration and concentration in vacuo provided 83.9 g of crude 32 as an oil which is used without further purification.To a solution of crude 32 in NMP (180 ml) was added potassium ferrocyanide(31.1 g, 84.44 mmol) and Na2CO3 (23.55 g, 222.2 mmol). The resulting slurry was degassed thoroughly via repeated evacuation and purging with nitrogen. The slurry was heated to about 100 C and a solution of Pd(OAc)2 (150 mg, 0.67 mmol) and DPPF (505 mg, 0.91 mmol) in degassed NMP (20 mL) added. The mixture was heated to ca. 130 C for about 3 h. HPLC analysis indicated ca. 5% starting material remained. Additional Pd(OAc)2 (50 mg, 0.22 mmol) is added and heating at 130 C was continued for 1.5 h when HPLC analysis showed complete conversion.After cooling toluene (400 mL) and saturated sodium sulfite solution (10 mL) are added and mixture heated at ca. 40 C for about 1 h. Solka-floc (10 g) was added and the mixture was filtered through a bed of Solka-floc and the cake was washed with toluene {ca. 100 mL total). The filtrate was washed successively with dilute sodium sulfite solution (1 x 400 mL) and water (2 x 200 mL). The combined aqueous phases are extracted with toluene (1 x 100 mL) and the toluene back extracted with water (2 x 50 mL). The combined organic phases are polish filtered, and concentrated in vacuo to obtain 70.4 g of 34 as a dark-colored oil (70.4 g) which was used in the next step without further purification.To the solution of crude 36 in toluene (190 mL) and anisole (65 mL) is added TFA (25.3 g, 222.2 mmol). The reaction was heated to ca. 65 C and stirred for about 2 h until the reaction was complete by HPLC. The mixture was distilled in vacuo to remove most of the TFA. After cooling, the mixture is extracted twice with ca. 10% Na2CO3 solution (300 mL then 150 mL). The combined aqueous phases were acidified to a pH of 5.5 with con HCl and extracted with EtOAc (2 x 200 mL). The combined organic phases were washed with water (1 x 150 ml), polish filtered and the solvent replaced with toluene by vacuum distillation. The solution was concentrated to ca. 200 mL, then heptane (200 mL) was slowly added and the mixture heated to 80 C. The mixture was cooled to RT, aged overnight, filtered, and washed with 50% heptane in toluene {ca. 30 mL). The isolated product was dried in vacuo at ca. 60 C to afford 29.0 g (77.2% yield over 3 steps)of 36.

The chemical industry reduces the impact on the environment during synthesis 1-Bromo-3-(difluoromethyl)-5-fluorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2008/145563; (2008); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 6698-13-1,Some common heterocyclic compound, 6698-13-1, name is 4-Bromo-1,3-benzodioxole, molecular formula is C7H5BrO2, 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.

[0154] A mixture of 2-chloro-5-methyl-pyrimidin-4-ylamine (1.4 g, 9.7 mmol), 4-bromo- benzo[l,3]dioxole (2.0 g, 10 mmol), Pd2(dba)3 (0.80 g, 0.87 mmol), Xantphos (1.0 g, 1.7 mmol) and cesium carbonate (6.3 g, 19 mmol) was suspended in dioxane (40 mL) and heated at reflux under the argon atmosphere for 5 h. The reaction mixture was cooled to room temperature and diluted with DCM (30 mL). The mixture was filtered and the filtrate concentrated in vacuo. The residue was purified by flash chromatography on silica gel (hexanes to 50% EtOAc/hexanes) to afford the title compound (1.0 g, 39%) as a white solid. 1H NMR (500 MHz, DMSO-d6): delta 2.13 (s, 3H), 5.99 (s, 2H), 6.80-6.90 (m, 3H), 8.01 (s, IH), 8.92 (s, IH). MS (ES+): m/z 264 (M+H)+.

The synthetic route of 6698-13-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TARGEGEN, INC.; WO2007/53452; (2007); 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. 392-83-6, name is 2-Bromobenzotrifluoride, A new synthetic method of this compound is introduced below., Recommanded Product: 392-83-6

General procedure: A DMF solution (8mL) of the o-substituted aryl iodide (0.36mmol), the o-bromobenzyl alcohol (0.36mmol) and norbornene (34mg, 0.36mmol) was added under nitrogen to a Schlenck-type flask, containing Pd(OAc)2 (4mg, 0.018mmol), the phosphine (0.036mmol), when required, and K2CO3 (124mg, 0.90mmol) or CsOPiv (211mg, 0.90). The reaction mixture was stirred at 105C for 24h. After cooling to room temperature the organic layer was diluted with EtOAc (20mL), washed twice with water (20mL) and dried over Na2SO4. The solvent was removed under reduced pressure and the resulting residue was purified by flash chromatography on silica gel using mixtures of hexane-EtOAc as eluent.

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; Della Ca, Nicola; Fontana, Marco; Xu, Di; Cremaschi, Mirko; Lucentini, Riccardo; Zhou, Zhi-Ming; Catellani, Marta; Motti, Elena; Tetrahedron; vol. 71; 37; (2015); p. 6389 – 6401;,
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. 73096-42-1, name is 5-(2-Bromophenyl)tetrazole, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C7H5BrN4

A suspension of [5-(2-BROMOPHENYL)-1 H-TETRAZOLE (4.] 50 [G] ; 20.0 [MMOL)] in ter-butyl methyl ether (40 ml) is warmed to [45C] and [METHANESULFONIC] acid (0.058 [G ;] 0.60 [MMOL)] is added. A solution of 3,4-dihydro-2H-pyran (1.90 ml ; 21 [MMOL)] in tert-butyl methyl ether (21 ml) is added to the resulting mixture over 1 hour at [45C.] The mixture is further stirred for 6 hours at [45C.] The resulting solution is cooled to about [0C] and a solution of sodium hydrogencarbonate (2.4 [G)] in water (30 ml) is added. The aqueous phase is separated and extracted with ter-butyl methyl ether (10 [ML).] The combined organic phases are washed twice with a 1 N KOH solution (10 mi each) and once with a solution of 10 weight-% of sodium chloride in water (10 ml). The resulting organic phase is dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to afford a mixture of [5- (2-BROMOPHENYL)-2-] [(TETRAHYDROPYRAN-2-YL)-2H-TETRAZOLE (N2-ISOMER)] and [5- (2-BROMOPHENY))-1- (TETRAHYDROPYRAN-] [2-YL)-1 H-TETRAZOLE (N1-ISOMER)] in a ratio of about 93: 7 (according [TO 1H-NMR) aS AN ORANGE] oil. 1H-NMR of N2-isomer [(400] MHz, CDCI3) : 1.72-1. 85 [(M,] 3 H), 2.18-2. 26 (m, 2 H), 2.45-2. 54 (m, 1 H), 3.80-3. 86 (m, 1 H), 4.01-4. [07] (m, 1 H), 6.12-6. 15 (m, 1 H), 7.31-7. 35 (m, [1] H), 7.41-7. 45 (m, [1] H), 7.73-7. 75 (m, 1 H), [7 :] 87-7.90 (m, 1 H).

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 73096-42-1.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2004/26847; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 128259-71-2, A common heterocyclic compound, 128259-71-2, name is 2,5-Dibromo-1,3-difluorobenzene, molecular formula is C6H2Br2F2, 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.

45 mL of an N-methylpyrrolidone suspension of 10.0 g (36.8 mmol) of 2,5-dibromo-1,3-difluorobenzene, 16.6 g (110.4 mmol) of 4-(tert-butyl)phenol, and 15.3 g (110.4 mmol) of K2CO3 was stirred at a temperature of 170 C. for 20 hours under a nitrogen atmosphere. The reaction mixture was diluted with toluene, and water was poured to extract an organic layer therefrom. The organic layer was washed with water, dried by using MgSO4, and filtered and concentrated by silica gel. The residue obtained therefrom was diluted with ethanol and filtered to obtain 15.7 g (80%) of Intermediate 1.

The synthetic route of 128259-71-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Samsung Display Co., Ltd.; Industry Academic Cooperation Foundation Kyunghee University; PARK, Miehwa; KWON, Janghyuk; KIM, Taekyung; LEE, Juyoung; JEONG, Hyein; AHN, Daehyun; SHIN, Daeyup; KIM, Siwoo; MOON, Jisu; (85 pag.)US2019/315776; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 5401-62-7, name is 1,2-Dibromocyclohexane, molecular formula is C6H10Br2, 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. category: bromides-buliding-blocks

General procedure: To a stirred solution of bisphenol (5/12) (1 mmol) in MeCN (15 mL) was added K2CO3 (5 mmol) and theresultant suspension was stirred for 30 min. Then, 1,6-dibromohexane (3 mmol) was added dropwise overa period of 10 min. Further, the crude reaction mixture was stirred for 12 h at reflux. At the conclusion ofthe reaction (TLC monitoring), the crude mixture was filtered through celite pad (washed with CH2Cl2)and concentrated under reduced pressure. The crude product was purified by column chromatography.Cyclophane products (7 and 18) data obtained by this procedure was compared with data obtained byhydrogenation process.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5401-62-7, its application will become more common.

Reference:
Article; Kotha, Sambasivarao; Waghule, Gopalkrushna T.; Heterocycles; vol. 90; 2; (2015); p. 1289 – 1298;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 1786-36-3, 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. 1786-36-3, name is (2-Bromo-1-fluoroethyl)benzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Under a nitrogen atmosphere, nickel bromide (4.4 mg, 0.02 mmol),4,4′-dimethyl-2,2′-bipyridine (3.68 mg, 0.02 mmol),Tetrabutylammonium iodide (14.77 mg, 0.04 mmol) manganese powder (43.95 mg, 0.8 mmol),Add solvent NMP (0.5 mL) and stir well.Weigh 4-bromobiphenyl (46.62mg, 0.2mmol) in NMP (0.5mL),After dissolution, add (2-bromo-1-fluoroethyl) benzene (60.92 mg, 0.3 mmol) and mix well.The solution was transferred to a sealed tube. After sealing, the reaction was stirred in an oil bath at 80 C for 24 hours.The reaction solution was cooled to room temperature, and an equal volume of a saturated ammonium chloride solution was added to the diluted reaction solution with ether (5 mL), filtered through a diatomaceous earth funnel, rinsed with a small amount of ether, and the filtrate was collected.The filtrate was extracted three times with diethyl ether, and the organic phases were combined (add internal standard dodecane,GC-MS determined crude yield). Dry over anhydrous sodium sulfate, filter, and remove the solvent by distillation under reduced pressure.After the residue was separated by silica gel column chromatography, the product was weighed.The calculated yield was 39%.

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-Bromo-1-fluoroethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sichuan Qing Chemical University; Yang Yi; Luo Gen; Li Youlin; Tong Xia; He Mengmeng; Jiang Yan; Liu Yingle; Shu Yumei; Zheng Yubin; Lu Wenjie; Zhao Yanchuan; (22 pag.)CN110803977; (2020); A;,
Bromide – Wikipedia,
bromide – Wiktionary