Month: January 2021

Reference of 402-43-7, The chemical industry reduces the impact on the environment during synthesis 402-43-7, name is 1-Bromo-4-(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

General procedure: Aniline ligand (10.0mmol) and palladium dichloride (0.886g, 5.0mmol) were dissolved in 15mL of DMAc at room temperature. After the mixture was stirred for 0.5hat 80C, the methanol (50mL) was added and the precipitation was formed. The precipitate of palladium complexes was then dissolved in 5mL dichloromethane, then 20mL hexane was added. After crystallized from the mixture of ethanol and dichloromethylene, the palladium complex was obtained as light yellow crystals.

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

Reference:
Article; He, Xiao-Xi; Li, Yan-Fang; Huang, Ju; Shen, Dong-Sheng; Liu, Feng-Shou; Journal of Organometallic Chemistry; vol. 803; (2016); p. 58 – 66;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 7073-94-1, name is 1-Bromo-2-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 7073-94-1, name: 1-Bromo-2-isopropylbenzene

1-Bromo-2-isopropylbenzene (15.0 g, 75.3 mmol),4-chlorophenylboronic acid (14.1 g, 90.4 mmol),Tetrakistriphenylphosphine palladium (1.74 g, 1.51 mmol),Potassium carbonate (20.8 g, 151 mmol),Tetrabutylammonium bromide 4.86 g, 15.1 mmol),Toluene (80mL),Ethanol (80 mL) and deionized water (80 mL) were added to a round bottom flask.Raise to 75-80 C under nitrogen atmosphere and stir for 16 hours;The reaction solution was cooled to room temperature, and toluene (150 mL) was added for extraction.The organic phases were combined, dried over anhydrous magnesium sulfate and filtered.The solvent is removed under reduced pressure;The obtained crude product was recrystallized and purified using a dichloromethane/n-heptane system.Intermediate I-B-1 (7.89 g, 45%) was obtained as a yellow solid.

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

Reference:
Patent; Shanxi Laite Optoelectric Materials Co., Ltd.; Ma Tiantian; Feng Zhen; Li Hongyan; Li Jian; Sha Xunshan; (37 pag.)CN110105225; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 167355-41-1, The chemical industry reduces the impact on the environment during synthesis 167355-41-1, name is 6-Bromo-1,2,3,4-tetrahydronaphthalen-2-amine, I believe this compound will play a more active role in future production and life.

Di-tert-butyldicarbonate (575.7 mg, 2.64 mmol) in methylene chloride (5.0 mL) is added in one portion to a solution of methylene chloride (7.0 mL) at room temperature that contains (rac)- 6-Bromo-l,2,3,4-tetrahydronaphthalen-2-ylamine (591.6 mg, 2.62 mmol) and triethylamine (1.1 mL, 7.89 mmol). After stirring at room temperature for 19 h in air, the resulting amber solution is diluted with methylene chloride (25 mL), washed with a saturated aqueous solution of sodium chloride (2 x 50 mL), dried over magnesium sulfate, and evaporated to dryness under reduced pressure to give the title compound as a pale yellow solid. The purity of isolated 29 was >95%, as determined by 1H NMR spectroscopy, and was used without further purification, mp 107-108 EPO C. 1H NMR (CDCl3): delta 1.45 (s, 9H, C(CH3)3), 1.70 (m, IH, H-3), 2.04 (m, IH, H-3), 2.55 (dd, J= 16.5 Hz, 8.5 Hz, IH, H-I), 2.84 (pseudo t, J= 6.5 Hz, 2H, H-4), 3.05 (dd, J= 16.5 Hz, 5.0 Hz, IH, H-I), 3.94 (br, IH, H-2), 4.58 (br, IH, NH), 6.91 (d, J= 8.0 Hz, IH, H-8), 7.22 (m, 2H, overlapping H-5 and H-7). 13C NMR (CDCl3): 527.1 (CH2, C-4), 28.4 (C(CH3)3), 28.7 (CH2, C- 3), 35.6 (CH2, C-I), 46.0 (CH, C-2), 79.4 (C(CHa)3), H9.6 (C-Br, C-6), 128.9 (CH, C-7), 131.0 (CH, C-8), 131.5 (CH, C-5), 133.3 (C-8a), 137.8 (C-4a), 155.3 (NHCO2). LCMS mk calcd for C15H20BrNO2 ([M]+) 325; found 311 ([M – C4H7 + CH3CN]+, 22%), 270 ([M – C4H7]+, 81%), 267 ([M – C5H7O2 + CH3CN]+, 43%), 226 ([M – C5H7Oa]+, 100%), 209 ([M – C5H10NO2]4″, 94%).

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-1,2,3,4-tetrahydronaphthalen-2-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ACHILLION PHARMACEUTICALS, INC.; WO2006/89054; (2006); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 50548-45-3, The chemical industry reduces the impact on the environment during synthesis 50548-45-3, name is 1-Bromodibenzo[b,d]furan, I believe this compound will play a more active role in future production and life.

Under an argon atmosphere, 1.00 g of Compound B, 2.81of 1 -bromodibenzothran, 0.27 g of bis(dibenzylideneac5 etone)palladium(0), 0.088 g of tri-tert-butylphosphine and3.98 g of sodium tert-butoxide were added to a 500 ml, three necked flask, followed by heating and refluxing in 200 ml oftoluene solvent for about 7 hours. After air cooling the resulting reactant, water was added to the reactant, an organic layer was separated therefrom, and solvents were distilled. The crude product thus obtained was separated using silica gel column chromatography (using toluene/hexane) to produce 1.90 g of Compound C as a white solid(Yield 70%). The molecular weight of Compound C thusobtained was measured using FAB-MS, and a value of 525 (C38H23N02) was obtained. In addition, the glass transition temperature of Compound C was measured using a differential scaiming calorimetry (DSC 7020 of Hitachi HightechCo.) and a value of 120 C. was obtained.

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-Bromodibenzo[b,d]furan, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Samsung Display Co., Ltd.; Miyake, Hideo; Takada, Ichinori; Nakano, Hiromi; (31 pag.)US10347844; (2019); B2;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 21120-91-2, A common heterocyclic compound, 21120-91-2, name is 7-Bromobicyclo[4.2.0]octa-1,3,5-triene, molecular formula is C8H7Br, 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.

General procedure: In a 250 ml three necked round bottom flask equipped with a polytetraflouroethylene (Teflon polymer, Dupont, Wilmington, Del.) coated magnetic stir bar, potassium hydroxide (1.38 g, 1 eq) was dissolved in water (6.83 g). Then 4-acetoxy styrene (4 g, 1 eq) was added dropwise at room temperature, and the solution turned from colorless to pale orange. Potassium carbonate (6.82 g, 2 eq) was added portionwise, and the solution was stirred for one hour. The flask was equipped with a reflux condenser, then 1-bromobenzocyclobutene (4.06 g, 1 eq) was added dropwise in DMF (41 ml). The solution was then heated to 70 C. and allowed to reflux overnight. To the reaction was added water (50 ml) and ethyl acetate (50 ml). The aqueous residue was extracted four times with ethyl acetate (100 ml). The combined organics were extracted with sodium bicarbonate solution (1¡Á100 ml), lithium chloride aqueous solution (1¡Á100 ml) and brine (2¡Á100 ml). The organics were dried over sodium sulfate, filtered and concentrated in vacuo to give the product as a of white solid (3.36 g, 68% yield). Melting point 54-60 C. 1H NMR (600 MHz, Chloroform-d) delta 7.39 (d, J=8.6 Hz, 2H), 7.34 (td, J=7.3, 1.5 Hiz, 1H), 7.31-7.24 (m, 2H), 7.21-7.18 (m, 1H), 6.98 (d, J=8.6 Hz, 2H), 6.69 (dd, J=17.6, 10.9 Hz, 1H), 5.70 (dd, J=4.3, 1.9 Hz, 1H), 5.64 (dd, J=17.6, 0.9 Hz, 1H), 5.15 (dd, J=10.9, 0.9 Hz, 1H), 3.73 (dd, J=14.2, 4.3 Hz, 1H), 3.31 (d, J=14.2 Hz, 1H). 13C NMR (151 MHz, Chloroform-d) delta 157.79, 144.62, 142.57, 136.20, 130.87, 129.93, 127.50, 127.43, 123.48, 123.04, 115.06, 111.80, 74.28, 39.45. Yield from the above example was good and the resulting monomer was a stable solid which has a desirable ring opening cure temperature of 184 C.

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; Rohm and Haas Electronic Materials LLC; Hayes, Colin; Gallagher, Michael K.; Riener, Michelle; (10 pag.)US2019/169327; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 314084-61-2, 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. 314084-61-2, name is 2-Bromo-1,3-diethyl-5-methylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution at -78C of 25g (110 mmol) of 2,6-diethyl-4-methylbromobenzene (preparation described in WO 2000078712) in 240 ml of tetrahydrofuran is added a -1.6 M solution of butyllithium in hexanes (75 ml, 120 mmol) dropwise over 10 minutes. The mixture is stirred for 10 minutes at -78cC, then trimethylborate (24.6 ml, 22.9g; 220 mmol) is added at once and stirring is continued at -780C for 30 minutes. The cooling bath is removed and the solution is allowed to warm up to room temperature over 1 hour and quenched with 2N aqueous hydrochloric acid (140 ml).The organic layer is separated, and the aqueous phase is extracted three times with diethyl ether : hexane 1 :1. The organic extracts are combined, dried over anhydrous sodium sulfate, filtered and the filtrate concentrated in vacuo. The oily residue is taken up in hexane under stirring, and the white solid is collected by filtration to give 2,6-diethyl-4-methylphenylboronic acid. The filtrate is concentrated and purified by column chromatography on silica gel give a further quantity of desired product. A combined yield of 16.6g (78%) of 2,6-diethyl-4-methylphenylboronic acid is obtained.

The synthetic route of 2-Bromo-1,3-diethyl-5-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; WO2008/110307; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 1435-51-4, 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. 1435-51-4, name is 1,3-Dibromo-5-fluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To mixture of 1,3-dibromo-5-fluorobenzene (LXXXV) (100 g, 393 mmol) and N’,N’-dimethylethane-1,2-diamine (173 g, 1.97 mol, 214 mL) was added t-BuOK (88 g, 787 mmol) in one portion at 25C under N2. The mixture was stirred at 25C for 30 min, then heated to 110C and stirred for 11.5 h. The mixture was cooled to 25C and concentrated in reduced pressure at 45C. The residue was purified by silica gel chromatography (column height: 250 mm, diameter: 100 mm, 100-200 mesh silica gel, PE/EtOAc = 2: 1, Rf = 0.6) to give N1-(3-bromo-5-fluorophenyl)-N2,N2-dimethylethane-1,2-diamine(LXXXVI) (30 g, 114.9 mmol, 29.2% yield) as a yellow oil. ESIMS found for C10H14BrFN2 m/z 261.1 (M+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, 1,3-Dibromo-5-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SAMUMED, LLC.; KC, Sunil, Kumar; WALLACE, David, Mark; CAO, Jianguo; CHIRUTA, Chandramouli; HOOD, John; (279 pag.)WO2017/23973; (2017); 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. 69038-76-2, name is 4-Bromo-N1-methylbenzene-1,2-diamine, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H9BrN2

Step 1: Synthesis of Intermediate 1-27.1 4-bromo-l-n-methylbenzene-l,2-diamine (4.42g, 21.98 mmol), N,N’-carbonyl-di-(l ,2,3-triazole (4.178g, 24.18 mmol), and TEA (9.184 mL, 65.95 mmol) in THF (70mL) are stirred at r.t. for 30min, then heated under reflux overnight. The reaction mixture is concentrated, triturated with water, filtered off and dried. The residue is triturated again with DIPE and filtered off. Yield 88%

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 69038-76-2.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; ANDERSKEWITZ, Ralf; GRAUERT, Matthias; GRUNDL, Marc; HAEBEL, Peter, Wilhelm; OOST, Thorsten; PAUTSCH, Alexander; PETERS, Stefan; BINDER, Florian; VINTONYAK, Viktor; WO2014/140075; (2014); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 73918-56-6, A common heterocyclic compound, 73918-56-6, name is 2-(4-Bromophenyl)ethanamine, molecular formula is C8H10BrN, 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 4-bromobenzeneethanamine (1.23 g, 6.17 mmol) and 2,6-lutidine (0.76 mL, 6.5 mmol) in dry CH2CI2 (25 mL) was cooled to 0 C. Trifluoroacetic anhydride (0.87 mL, 6.2 mmol) was added dropwise, and the reaction was then warmed to room temperature and allowed to stir for 16 h. Water (25 mL) was added to the reaction, the phases were separated, and the aqueous layer was extracted with CH2C12 (2 x 25 mL). The combined organic phases were washed successively with 1 M HCl (25 mL) and saturated NaHCO3 (25 mL), and then dried over NA2S04, filtered, and concentrated in vacuo to provide the title compound (1.79 g, 98%). The crude compound was used in subsequent STEPS.’H-NMR (CDC13); 8 7.49-7. 45 (m, 2H), 7.10-7. 06 (m, 2H), 6.27 (br s, 1H), 3.61 (q, J=6. 8 Hz, 2H), 2.86 (T, J=6. 8 Hz, 2H). MS (ESI) (M+H) += 296/298.

The synthetic route of 73918-56-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2004/60882; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 1435-52-5, 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. 1435-52-5, name is 1,4-Dibromo-2-fluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 1,4-dibromo-2-fluorobenzene (6.86 g, 27 mmol), ethanediol (35 mL), N-methylpyrrolidone (35 mL) and potassium tert-butoxide (11.2 g, 95 mmol) was stirred at 100 C overnight under N2. After the mixture was cooled to room temperature, water (15 mL) was added slowly within 30 min. Then the mixture was filtered, and the filter cake was washed by ethanediol. To the filtrate was added water and the mixture was stirred for 30 min. The resulting solution was then cooled to 15 C, and let stay for 1 h. The precipitate was filtered, washed by water, and dried to give the title compound (4.70 g, 59 %). 1H NMR (CDCl3): delta 7.40 (1H, d, J = 8.4 Hz), 7.05 (1H, d, J = 2.4 Hz), 7.02-6.70 (1H, m), 4.14 (2H, t, J = 4.4 Hz), 4.02-3.98 (2H, m), 2.13 (1H, t, J = 6.4 Hz)

The synthetic route of 1,4-Dibromo-2-fluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Li, Yuliang; WANG, Huting; ZHU, Yan; WANG, Zhe; ZHANG, Hui; ZHAO, Ruiyu; HUANG, Yuanyuan; WANG, He; PENG, Yong; LUO, Hong; XIAO, Dengming; CAO, Shousong; HAN, Yongxin; EP2862571; (2015); A1;,
Bromide – Wikipedia,
bromide – Wiktionary