Author: Jessica.F

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. name: 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 66417-30-9, These common heterocyclic compound, 66417-30-9, name is 2-Bromo-1-methyl-4-(trifluoromethyl)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.

A solution of 2-bromo-1-methyl-4-(trifluoromethyl)benzene (4.78 g, 20 mmol) in 100 mL of anhydrous THF was cooled to -100 C (liquid nitrogen/ EtOH) under nitrogen. Then 1.4M solution of sec-BuLi in cyclohexane (15 mL, 21 mmol) was added dropwise at – 100 C to -90 C. The mixture was stirred at -100 C to -90 C for 10 min, then a solution of R-(+)-propylene oxide (1.51 g, 1.8 mL, 26 mmol) in 15 mL of THF was added dropwise at -100 C to -90 C, then the mixture was cooled to -105 C and a 46.5% solution Of BF3 in diethyl ether (4.18 mL, 30 mmol) was added dropwise. The mixture was stirred at -100 C to -90 C for 2 h, then the reaction was quenched with 20 mL of sat. aq. NH4Cl at -90 C. The mixture was stirred and warmed to 0 C overnight. Then 20 mL of water was added and mixture was extracted with EtOAc (2×60 mL), the extract was dried over Na2SO4 and evaporated to give crude oil, which was purified by column (silicagel, EtOAc/hexane 1 :9, Rf = 0.45 in EtOAc/hexane 3:7) to give (2R)-1-[2- methyl-5-(trifluoromethyl)phenyl]propan-2-ol (2.87 g, 66 %) as white solid. 1H NMR (300 MHz, CDCl3): delta 7.42 (s, 1H), 7.39 (d, J = 8.1 Hz, 1H), 7.27 (d, J = 8.1 Hz, 1H), 4.06 (m, 1H), 2.81 (d, J = 6.39 Hz, 2H), 2.39 (s, 3H), 1.43 (d, J = 4.14 Hz, 1H), 1.29 (d, J = 6.21 Hz, 3H).

The synthetic route of 66417-30-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CHEMBRIDGE CORPORATION; WO2009/117097; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 60956-23-2, A common heterocyclic compound, 60956-23-2, name is 1,2-Dibromo-4-methylbenzene, molecular formula is C7H6Br2, 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.

Add 4-methyl-o-dibromobenzene (1.0 mmol), tBuOOH (1.5 mmol), andCu (acac) 2 (0.06mmol), then add 2mL of solvent water, and react at room temperature for 10 hours,After the reaction was completed, the reaction solution was concentrated, and the corresponding product was obtained by column chromatography. The isolated yield was 93%.

The synthetic route of 60956-23-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Institute of Technology; Yao Zijian; Qiao Xinchao; (6 pag.)CN110981702; (2020); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature 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

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. 82842-52-2, name is 3-Bromo-2,4,6-trimethylaniline, A new synthetic method of this compound is introduced below., SDS of cas: 82842-52-2

Second Step To a solution of 3-bromo-2,4,6-trimethylaniline (2.0 g, 9.18 mmol) in DMSO (25 mL) was added iodoethane (1.86 mL, 44.9 mmol) and potassium carbonate (5.06 g, 36.6 mmol), and the solution was heated to 60 C. for 16 hours and cooled to room temperature. The mixture was diluted with ethyl acetate (300 mL), washed with saturated NaCl (2*), and dried over magnesium sulfate. The solvent was removed under reduced pressure. The crude product was purified by column chromatography (silica gel) with hexane/ethyl acetate as the mobile phase to give 1-(N,N-diethylamine)-3-bromo-2,4,6-trimethylbenzene (4.0 g, 54%). as a colorless liquid.

The synthetic route of 82842-52-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wu, Chengde; Anderson, C. Eric; Bui, Huong; Gao, Daxin; Kassir, Jamal; Li, Wen; Wang, Junmei; Biediger, Ronald; Chen, Jie; Market, Robert V.; US2005/49286; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application 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

Related Products 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

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. 6274-57-3, name is 1-(4-Bromophenyl)-N,N-dimethylmethanamine, A new synthetic method of this compound is introduced below., Computed Properties of C9H12BrN

General procedure: At room temperature, organic carbonyl acid 3 (R-COOH, 0.5 mmol) was added into a reaction tube equipped with a small magnet. Then a solution of tertiary amine 1 (R1CH2-NR2R3, 0.5 mmol ) in DCM (2.5 mL) was added dropwise in 2 min. After the mixture was stirred at room temperature for a few minutes, 1 equivalents of dimethyl acetylenedicarboxylate (DMAD, 2) was added. The reaction was stirred overnight at room temperature, and then monitored by TLC with silica gel coated plates. After being stirred for 14 h, the solvent was removed and the residue was purified by a flash column chromatography with silica gel with ethyl acetate/hexane (1:25-30) as eluent to give the desired products 4, 5, and 7. Most of compounds are known and confirmed by NMR, ESI-MS, IR.

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; Shen, Hao; Lu, Xing; Jiang, Ke-Zhi; Yang, Ke-Fang; Lu, Yixin; Zheng, Zhan-Jiang; Lai, Guo-Qiao; Xu, Li-Wen; Tetrahedron; vol. 68; 43; (2012); p. 8916 – 8923;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 399-94-0,Some common heterocyclic compound, 399-94-0, name is 1-Bromo-2,5-difluorobenzene, molecular formula is C6H3BrF2, 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.

Under the protection of nitrogen, 2,5-difluorobromobenzene (15.05g, 78mmol) is dissolved in dry toluene (50 ml), lowering the temperature to ice salt bath -10 C following, dropwise adding isopropyl magnesium chloride/tetrahydrofuran solution of lithium chloride (66 ml, 1.3 mol/L), maintained at about -10 C stirring 1 hour. the1D (10g, 39mmol) dissolved in dry tetrahydrofuran (100 ml) in, is dropped is added to the reaction solution, maintaining the temperature -10 C, canada finishes, to react at room temperature for 4 hours. The temperature dropped to about -10 C, dropwise adding saturated ammonium chloride solution (40 ml), stirring 10 minutes, for 3 mol/L hydrochloric acid solution to adjust pH value to 5 – 6, layered, 3rd phase for methyl tert-butyl ether (50mL × 2) extraction, the combined organic phase, saturated sodium chloride solution (30mL × 2) washing, drying of the organic phase by adding anhydrous sodium sulfate, filtered, concentrated, column chromatography (petroleum ether/ethyl acetate=50:1 – 8:1 (v/v)), get the yellow solid1E(10.1g, 83.5% yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2,5-difluorobenzene, its application will become more common.

Reference:
Patent; SICHUAN HAISCO PHARMACEUTICAL CO., LTD; ZHANG, CHEN; FAN, JIANG; LI, CAI-HU; WEI, YONG-GANG; (99 pag.)TW2017/8222; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products 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