Month: September 2021

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. 445-02-3, name is 4-Bromo-2-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H5BrF3N

A. 2-Acetamido-5-bromobenzotrifluoride A solution of 2-amino-5-bromobenzotrifluoride (1.623 g, 6.76 mmol, Aldrich) in acetic anhydride (10 mL) was stirred at room temperature for 12 h to produce a white needle precipitate. It was filtered to give 1.840 g (99.7%) of title compound. Mp: 140-2 C., 1 H-NMR (CDCl3): delta2.212 (s, 3H); 7.358(s, 1H); 7.659(d, 1H, J=8.7 Hz); 7.726(d, 1H, J=1.8 Hz); 8.118 (d, 1H, J=8.4 Hz).

The synthetic route of 445-02-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; The State of Oregon, acting by and through The Oregon State Board of Higher Education, acting for and on behalf of The Oregon Health Sciences University; The University of Oregon; The Regents of the University of California; US5514680; (1996); A;,
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. 5469-19-2, name is 1-Bromo-2,4,5-trimethylbenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 5469-19-2

1-Bromo-2,4,5-trimethylbenzene (25.0 g, 0.125 mol) was dissolved in methylene chloride (500 mL). Aluminum chloride (20.1 g, 0.151 mol) and dichloromethyl methyl ether (13.7 mL, 0.151 mol) were added in a nitrogen atmosphere at -78C. After stirring at -78C for five minutes, water (500 mL) was added, followed by extraction with methylene chloride (400 mL). The organic layer was washed with brine and then dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate = 25/1) to give the target compound (14.4 g, yield: 51%) as a white solid. 1H-NMR (CDCl3, 400MHz):delta ppm: 2:27 (3H, s), 2.36 (3H, s), 2.55 (3H, s), 7.51 (1H, s), 10.53 (1H, s). MS (EI) m/z: 226 (M+)

The synthetic route of 5469-19-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daiichi Sankyo Company, Limited; EP1914229; (2008); 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 33070-32-5 as follows. Safety of 5-Bromo-2,2-difluorobenzodioxole

To the dry reaction tankIn sulfolane 940g,Lithium bromide 130g,130g of cuprous cyanide was stirred evenly so that lithium bromide and cuprous cyanide dissolved, and then added5-Bromo-2,2-difluoro pepper ring 237g,The reaction was incubated at 135 8h,After the reaction was cooled to 20 C, water 2.9kg,Steam distillation of solid products, after drying 167g,The content of 167 g of 5-cyano-2,2-difluoro pepper ring was 99.3%, yield 91.2%.

According to the analysis of related databases, 33070-32-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Fuxin Aoruikai New Materials Co., Ltd.; Liu Min; Yang Yinxing; Chen Li; Liu Chunyu; Liu Wei; Qin Wenyi; (5 pag.)CN105153106; (2017); B;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 2789-89-1,Some common heterocyclic compound, 2789-89-1, name is 1,2-Bis(4-bromophenyl)ethyne, molecular formula is C14H8Br2, 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.

In 25mL dry pressure reaction tube, was added 58mg of 1-octyl-4- (p-chlorophenyl) -1,2,3-triazole, 134mg of 1-phenyl-1-propyne, 6mg of dichloro (pentamethylcyclopentadienyl yl) rhodium dimer, 80mg of copper acetate monohydrate, 32mg 1.5mL sodium peroxide and 1,2-dichloroethane.100 stirred for 24 hours.After the reaction was cooled to room temperature, directly on a silica gel column (ethyl acetate and petroleum ether, the volume ratio of 1: 3) to give product 48mg, 39% yield,

The synthetic route of 2789-89-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang University; Chen, Wanzhi; (11 pag.)CN104725375; (2016); B;,
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. 68322-84-9, name is 2-Bromo-1-fluoro-4-(trifluoromethyl)benzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 68322-84-9

3-Bromo-4-fluorobenzotrifluoride (0.38 mL, 2.67 mmol), Cs2C03 (1.74 g, 5.34 mmol), X-Phos (207 mg, 0.036 mmol) and Pd2(dba)3 (164 mg, 0.18 mmol), were added to a mixture of intermediate 31 and intermediate 32 (510 mg, 1.78 mmol) in 2-methyl-2- propanol (40 mL) under a N2 atmosphere. The r.m. was heated at 100 C for 16 h. Then, the r.m. was cooled to r.t., water was added and the r.m. was extracted with DCM. The combined organic layers were dried (MgS04), filtered and concentrated in vacuo. The residue was purified by flash column chromatography (eluent: DCM/MeOH from 100/0 to 95/5). The product fractions were collected and concentrated in vacuo. Both residue was suspended in DIPE and treated with a 6 N HC1 sol. in 2-propanol. Resulting precipitates were collected by filtration. The first compound impure was repurified by RP preparative HPLC [RP Vydac Denali CI 8 – IotaOmicronmu?iota, 250 g, 5cm); mobile phase: a gradient of (0.25% H4HC03 sol. in water/CH3CN)]. The product fractions were collected and concentrated in vacuo. Both residue was crystallized from DIPE, filtered off and dried. Yield: 118 mg of compound 11 (13 %) as HC1 salt (.HC1 .H20) and 97 mg of compound 11a (12 %; regioisomer of compound 11).

The synthetic route of 68322-84-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICALS, INC.; BISCHOFF, Francois, Paul; VELTER, Adriana, Ingrid; VAN BRANDT, Sven, Franciscus, Anna; BERTHELOT, Didier, Jean-Claude; WO2012/126984; (2012); 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. 583-75-5, name is 4-Bromo-2-methylaniline, A new synthetic method of this compound is introduced below., Product Details of 583-75-5

Adding the compound 183a (1.0 g, 5.37 mmol),Compound 183b (2.73 g, 10.75 mmol),Potassium acetate (1.58 g, 16.12 mmol) and PdCl2 (dppf) (0.39 g, 0.54 mmol) were added to 1,4-dioxane (20 mL), replaced with nitrogen three times, and then stirred at 90 C for 4 hours. The reaction solution was cooled to room temperature and filtered.The filter cake was washed with ethyl acetate (15 mL × 2), and the filtrate was concentrated.The concentrate was purified by silica gel chromatography (ethyl acetate: petroleum ether = 0-80%) to obtain a compound 183c as a yellow solid, namely , 2-Dioxoranepentyl-2-yl) aniline (1.21 g, 96.6% yield).

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; Jiaxing Tekeluo Biological Technology Co., Ltd.; Xing Li; Li Guanqun; Wang Xiaolei; Cai Yuting; Jiang Xiang; Pan Xiang; Zhu Wenhao; Wang Yang; Wang Zengquan; (83 pag.)CN110627775; (2019); A;,
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 5153-40-2 as follows. SDS of cas: 5153-40-2

General procedure: A mixture of aryl silane (0.5 mmol), aryl bromides (0.5 mmol), PdCl2(MeCN)2 (5 mol%), and CsF (0.5 mmol) was stirred at 100oC for 6 h in NMP under CO (1atm) (5 mL). Afterwards, 2 mL water was added to the reaction solution and then filtered through a filter paper and the solution was extracted by Et2O (2 mL) for three times. The organic phase was combined and evaporated under reduced pressure. The residue was purified on a SiO2 column to afford the desired product(ethyl acetate/hexane).

According to the analysis of related databases, 5153-40-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Chang, Sheng; Jin, Ying; Zhang, Xiu Rong; Sun, Yong Bing; Tetrahedron Letters; vol. 57; 19; (2016); p. 2017 – 2020;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 1422-53-3, 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. 1422-53-3, name is 2-Bromo-4-fluorotoluene, This compound has unique chemical properties. The synthetic route is as follows.

2-bromo-4-fluorotoluene (98 mg, 0.5 mmol),Carbon tetrabromide (16mg, 0.05mmol) was addedInto a reaction flask filled with oxygen,Plug in an oxygen balloon,Finally add 10ml of acetonitrile,Reaction at 400nm LED wavelength and room temperature for 60h,After the reaction, the solvent was distilled off under reduced pressure.Add excess 2mol / L sodium hydroxide solution for washing,Adjust the pH to about 10 ~ 11,The aqueous phase was extracted multiple times with ethyl acetate,Then add 2mol / L of dilute hydrochloric acid to the water phase,Adjust the pH to 1-2,The aqueous phase was extracted again with ethyl acetate several times,Evaporate the ethyl acetate and dry,That gives compound 22,The yield was 78.5%.

The chemical industry reduces the impact on the environment during synthesis 2-Bromo-4-fluorotoluene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Zhejiang University of Technology; Li Xiaoqing; Zheng Kun; Xu Xiangsheng; (26 pag.)CN110563571; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 626-40-4, 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 626-40-4 as follows.

Compound II (2.52 g, 10 mmol), compound III (2.51 g, 10 mmol) and diisopropylethylamine (DIPEA,3.88 g, 30 mmol) was dissolved in 50 mL of dry xylene and refluxed under nitrogen atmosphere until the reaction was completeUsually 5 hours). The reaction mixture was carefully poured into 200 mL of ice water, stirred, extracted with 50 mL of X3CH2C12, the combined phases were combined,Washed successively with 1% dilute hydrochloric acid (200 mL) and brine (100 mL), and dried over anhydrous sodium sulfate. The desiccant was removed by suction filtrationEvaporated on a rotary evaporator to give compound IV, a white solid.

According to the analysis of related databases, 626-40-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Guangdong Sai Bo Technology Co., Ltd.; Guo Huijun; (11 pag.)CN106831835; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 6274-57-3, These common heterocyclic compound, 6274-57-3, name is 1-(4-Bromophenyl)-N,N-dimethylmethanamine, 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.

Magnesium strips (0.36 g, 15 mmol), a small amount of iodine, 4-bromo-N,N-dimethylbenzylamine (0.21 g, 1 mmol), tetrahydrofuran (25 mL) were added to a round bottom flask, and the mixture was heated to reflux. The reaction is initiated.A solution of 4-bromo-N,N-dimethylbenzylamine (2.98 g, 14 mmol) in THF (5 mL) was then added dropwise over 30 min.After the addition is completed, the reflux is continued for 2 hours.Then cooled to room temperature, and slowly added the compound a derived from amino acid within 30 min.(2-[(tert-Butoxycarbonyl)amino]-3-phenylpropanoic acid methyl ester) (1.40 g, 5 mmol) in THF (5 mL)The saturated ammonium chloride solution was quenched, extracted with ethyl acetate and washed with saturated brine.After drying over anhydrous sodium sulfate, a crude Boc-protected amino alcohol b was obtained, which was used directly in the next step.

The synthetic route of 6274-57-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; University of Science and Technology of China; Wang Zhiyong; Gui Yang; (28 pag.)CN108821995; (2018); A;,
Bromide – Wikipedia,
bromide – Wiktionary