Month: August 2021

Adding a certain compound to certain chemical reactions, such as: 57946-63-1, name is 2-Bromo-4-(trifluoromethyl)aniline, 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 57946-63-1, Recommanded Product: 2-Bromo-4-(trifluoromethyl)aniline

This compound was prepared by application of the procedure for oxidation of4-(trifluoromethyl)aniline.[7] A 300 mL three-necked round-bottom flask equipped with a refluxcondenser and a dropping funnel was charged with sodium perborate tetrahydrate (40.69 g, 0.264mol) and glacial acetic acid (50 mL). The dropping funnel was charged with2-bromo-4-(trifluoromethyl)aniline (6.31 g, 26.8 mmol) and glacial acetic acid (50 mL). Thesuspension in the flask was heated to 55°C and the content of the funnel was added dropwise to it.After 3 h, an additional sodium perborate tetrahydrate (20.00 g, 0.130 mol) was added to the reactionmixture and stirred at 55°C for 4 h. The resulting yellow suspension was cooled to room temperatureand filtered through a Celite pad. To the filtrate was added diethyl ether (200 mL) and water (100mL). The organic phase was separated from the mixture and aqueous phase was extracted withdiethyl ether (150 mL x 2). Combined organic phase was neutralized by aqueous sodium hydroxidesolution (3 M) and separated. The separated organic phase was dried over sodium sulfate andconcentrated to afford brown liquid. This crude product was purified by flash columnchromatography (12percent EtOAc/hexane) to give the title compound as a yellow liquid (4.22 g, 60 percent).

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:
Article; Takahashi, Hirotsugu; Watanabe, Takahito; Tobita, Hiromi; Chemistry Letters; vol. 47; 3; (2018); p. 296 – 299;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 17247-58-4, The chemical industry reduces the impact on the environment during synthesis 17247-58-4, name is (Bromomethyl)cyclobutane, I believe this compound will play a more active role in future production and life.

A stirred solution of ketimine 2a (50 g, 187.1 mmol) under N2 in dry THF (400 mL) was cooled to -78 C. and treated with 1 M solution of K-tBuO (220 mL, 1.15 equiv.) in THF. The reaction mixture was warmed to 0 C. and stirred for 1 h and treated with bromomethyl cyclobutane (28 mL, 249 mmol). The reaction mixture was stirred at room temperature for 48 h and concentrated in vacuo. The residue was dissolved in Et2O (300 mL) and treated with aq. HCl (2 M, 300 mL) The resulting solution was stirred at room temperature for 5 h and extracted with Et2O (1 L). The aqueous layer was made basic to pH 12-14 with NaOH (50% aq.) and extracted with CH2Cl2 (3×300 mL). The combined organic layers were dried (MgSO4), filtered, and concentrated to give the pure amine (2b, 18 g) as a colorless oil.

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, (Bromomethyl)cyclobutane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SCHERING CORPORATION; US2005/197301; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 4549-33-1, 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. 4549-33-1, name is 1,9-Dibromononane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Take a 50 mL flask, install a reflux condenser, and add 2.0 mL (12.56 mmol) of 2,3,3-trimethyl-3H-indole.2.55 mL of 1,9-dibromodecane (12.56 mmol) and 20 mL of tetrahydrofuran, heated to reflux for 24 hours;Stop heating and allow the reaction system to cool to room temperature;704.7 mg (12.56 mmol) of potassium hydroxide and 2.1 g (12.56 mmol) of 5-nitrosalicylaldehyde were sequentially added to the above system, and the reaction was further continued for 10 minutes.The system is neutralized with acid, washed, extracted, and the solvent is dried.The product was purified by silica gel column chromatography (eluent petroleum ether / ethyl acetate).A yellow solid was obtained in an amount of 1.93 g, yield 30%.

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, 1,9-Dibromononane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Qingdao University of Science and Technology; Deng Yawen; Xie Congxia; Wu Zhongtao; Zhang Lei; (6 pag.)CN110028517; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 69321-60-4, 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. 69321-60-4, name is 2,6-Dibromotoluene, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of 2,6-dibromotoluene (22.9 g, 92 mmol), N-bromosuccinimide (NBS) (15 g, 84 mmol), CC14 (250 mL) and benzoyl peroxide (0.03 eq) was stirred at 85C (hot oil bath temperature) for 16 h, cooled to RT, filtered, washed with aq. NaHS03, dried (Na2S04), filtered, and evaporated to give 29.5 g (yield of 98%>) of title product as a white solid. This solid contained 10% unreacted starting material but was successfully used without further purification. 1H NMR (300 MHz, CDC13) delta 4.81 (s, 2 H), 7.01 (t, 1 H), 7.53 (d, 2 H).

The chemical industry reduces the impact on the environment during synthesis 2,6-Dibromotoluene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF MICHIGAN; GLICK, Gary, D.; HURD, Alexander, Ross; VAN HUIS, Chad, Alan; WO2011/35124; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 18599-22-9, name is 4-Bromo-3,3,4,4-tetrafluorobut-1-ene, 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 18599-22-9, COA of Formula: C4H3BrF4

General procedure: In a two-necked round-bottomed flask, equipped with a teflon-coated stirrer bar and reflux condenser, was added ethyl 2-iodobenzoate (3j, 0.14 g 0.50 mmol), Cu2O (0.060 g, 0.42 mmol), and a DMF solution of 2-Zn (0.65 M, 1.54 mL, 1.0 mmol), and the mixture was stirred at 100 C for 24 h. After being cooled to room temperature, the resulting solution was subjected to a short pad of silica gel using hexanes as an eluent. The filtrate was concentrated in vacuo to give the crude materials, which was purified by silica gel column chromatography to provide the corresponding compound 4j (0.13 g, 0.48 mmol) in 96% yield as an yellow oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-3,3,4,4-tetrafluorobut-1-ene, and friends who are interested can also refer to it.

Reference:
Article; Tamamoto, Ken; Yamada, Shigeyuki; Konno, Tsutomu; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 2375 – 2383;,
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. 3814-30-0, name is (Bromomethyl)cyclopentane, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of (Bromomethyl)cyclopentane

General procedure: The alkyl bromide (1.0 equiv) was added to a solution of mercaptoaceticacid (1.0 equiv) in methanol (10.0 mL) and the resultingsolution stirred. Then a solution of NaOH (2.0 equiv) in methanol(5.0 mL)was added slowly, and the final mixturewas stirred at roomtemperature or heated to reflux until absence of the alkyl bromide(checked by TLC). The reaction mixture was concentrated in vacuo,diluted with H2O, and neutralized with 1 N HCl. Then the obtainedreaction mixture was extracted with EtOAc. The combined organicfractions were washed with brine, dried with Na2SO4, and concentratedin vacuo. Purification of the crude residue by column chromatography(petroleum ether/EtOAc) afforded the title compound.

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 3814-30-0.

Reference:
Article; Chen, Ying; Wu, Bolin; Hao, Yameng; Liu, Yunqi; Zhang, Zhili; Tian, Chao; Ning, Xianling; Guo, Ying; Liu, Junyi; Wang, Xiaowei; European Journal of Medicinal Chemistry; vol. 171; (2019); p. 420 – 433;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 112734-22-2, name is (4-Bromo-2-fluorophenyl)methanamine, 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 112734-22-2, Product Details of 112734-22-2

(2) To a solution of 4-bromo-2-fluorobenzylamine (0.93 g) and triethylamine (1.3 ml) in N,N-dimethylformamide (5 ml) was added a solution of ethyl (R)-2,5-dioxo-3-(2-trichloroacetylpyrrol-1-yl)pyrrolidine-3-carboxylate (1.16 g) in N,N-dimethylformamide (3 ml) dropwise at room temperature. This mixture was stirred at room temperature for 8 hours. This reaction mixture was diluted with ethyl acetate, then washed with 1M hydrochloric acid (three times), water (four times), and saturated brine successively, dried over magnesium sulfate, filtered and concentrated to give a crude product as yellow oil. This was purified by flash column chromatography (n-hexane:ethyl acetate=2:1) to give (3R)-2′-(4-bromo-2-fluorobenzyl)spiro[pyrrolidine-3,4′(1’H)-pyrrolo[1,2-a]pyrazine]-1′,2,3′,5(2H’)-tetraone (831 mg, 65%). This product was further crystallized from n-hexane-ethyl acetate to give the desired product (385 mg) as crystal.Mp: 189-191 C. 1H NMR (400 MHz, DMSO-d6, 22 C.) delta: 12.2 (br s, 1H), 7.73 (dd, 1H, J=2.0, 3.2 Hz), 7.55 (dd, 1H, J=2.0, 9.6 Hz), 7.36 (dd, 1H, J=2.0, 8.4 Hz), 7.17-7.12 (m, 2H), 6.53 (dd, 1H, J=2.8, 4.0 Hz), 5.04 (d, 1H, J=15.2 Hz), 4.96 (d, 1H, J=15.6 Hz), 3.57 (s, 2H).

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; Tanaka, Daisuke; US2009/253917; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Synthetic Route of 10016-52-1, A common heterocyclic compound, 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan, molecular formula is C12H6Br2O, 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.

Example 10 Synthesis of Compound 5 To a 20 mL DMSO solution of 2,8-dibromodibenzofuran (1 g, 3.07 mmol) was added bispinacolatiodiboron (1.74 g, 6.75 mmol), KOAc (2 g, 21 mmol) and PdCl2(PPh3)2 (149 mg, 0.21 mmol), and the solution was stirred at 80 C. for 24 h. The catalyst was removed by filtration and washed with CH2Cl2 after the reaction mixture was cooled to room temperature. The filtrate was then washed with de-ionized H2O (50 mL) for five times, and the organic layer was dried over Mg2SO4, filtrated, concentrated and purified by column chromatography on silica gel (hexane/EtOAc=10:1) to give 2,8-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)dibenzofuran (0.4 g, 31%). 1H NMR (400 MHz, CDCl3) delta 8.51 (s, 2H), 7.92 (d, 2H), 7.57 (d, 2H), 1.40 (s, 24H).

The synthetic route of 10016-52-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GENERAL ELECTRIC COMPANY; US2009/289224; (2009); 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. 4101-68-2, name is 1,10-Dibromodecan, A new synthetic method of this compound is introduced below., Computed Properties of C10H20Br2

General procedure: For example, to a solution of 7-hydroxycoumarin (5.0 g, 31.0 mmol) in acetone (60.0 mL) was added anhydrous K2CO3 (6.9 g, 50.0 mmol) and triethylamine (1.0 mL) at room temperature. After stirring at room temperature for 30 min, 1, 2-dibromoethane (12.6 g, 62.0 mmol) was added to the reaction mixture, and the whole was refluxed at 60C for 24 h. Then the reaction mixture was filtered, and the filtrate was evaporated under reduced pressure. The residue was treated with water (200.0 mL) and extracted with dichloromethane (4×200.0 mL). The organic layer was combined, dried with anhydrous Na2SO4, and concentrated under reduced pressure. The crude product was purified via silica gel column chromatography with mixed petroleum ether and ethyl acetate (5:1, v/v) as eluent, and resulted in a white solid.

The synthetic route of 4101-68-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Hu, Yang; Chen, Weichao; Shen, Yufeng; Zhu, Bin; Wang, Gao-Xue; Bioorganic and Medicinal Chemistry Letters; vol. 29; 14; (2019); p. 1749 – 1755;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 74586-53-1, 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. 74586-53-1, name is 3-Bromo-5-methylaniline, This compound has unique chemical properties. The synthetic route is as follows.

Preparative Example 1.2 – N-(3- opropylpyrimidin-2-amine [00216] To a solution of 2-chloro-4-cyclopropyl-pyrimidine (12.5 g, 81 mmol) and 3- bromo-5-methylaniline (18.1 g, 97 mmol) in 1,4-dioxane (100 mL) was added pivalic acid (9.3 mL, 81 mmol). The resulting mixture was heated to reflux and left stirring for 10 hours. The mixture was allowed to cool to room temperature and hexanes were added (80 mL). The slurry was filtered and the filtrate was washed with MeOH to afford a portion of N-(3-bromo-5- methylphenyl)-4-cyclopropylpyrimidin-2-amine. The mother liquors were concentrated, absorbed on silica gel and purified by silica gel column chromatography (EtO Ac/Hex) to afford additional N-(3-bromo-5-methylphenyl)-4-cyclopropylpyrimidin-2-amine as a white solid. MS ESI calc’d for Ci4H15BrN3 [M+H]+ 304 and 306, found 304 and 306.

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

Reference:
Patent; MERCK SHARP & DOHME CORP.; HAIDLE, Andrew, M.; ALTMAN, Michael, D.; KATTAR, Solomon, D.; CHRISTOPHER, Matthew; ELLIS, John, Michael; FISCHER, Christian; NORTHRUP, Alan, B.; CHILDERS, Kaleen Konrad; WO2013/192088; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary