Month: July 2021

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. 344-04-7, name is 1-Bromo-2,3,4,5,6-pentafluorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 344-04-7

General procedure: To a solution of halogenbenzene 1 (50mmol) in EtOH (30mL) was added hydrazine monohydrate (5.0g, 0.1mol). The reaction mixture was refluxed for 1÷20h (see Scheme 1), cooled to r.t., poured into H2O (100mL) and kept at 5C for 3h. The precipitate was filtered and recrystallized from hexane.

According to the analysis of related databases, 344-04-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Politanskaya, Larisa; Bagryanskaya, Irina; Tretyakov, Evgeny; Journal of Fluorine Chemistry; vol. 214; (2018); p. 48 – 57;,
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. 149910-98-5, name is 7-Bromoisochroman, A new synthetic method of this compound is introduced below., Computed Properties of C9H9BrO

General procedure: Toa solution of the substituted isochroman (7.46 mmol) derivatives inacetonitrile (15 ml), CuBr2(8.95 mmol)was added under nitrogenatmosphere. The solution was refluxed for about 2hr and then cooled to roomtemperature. The reaction mixture was added water, extracted with ethyl acetate.The combined organic extracts were washed with brine and dried with anhydrousNa2SO4,filtered and concentrated and then purified by silicagel column chromatographyto afford the product 1in 68% 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:
Article; Shinde, Anand H.; Archith; Malipatel, Srilaxmi; Sharada, Duddu S.; Tetrahedron Letters; vol. 55; 50; (2014); p. 6821 – 6826;,
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. 627871-16-3, name is 5-Bromo-4-fluoro-2-methylaniline, A new synthetic method of this compound is introduced below., Quality Control of 5-Bromo-4-fluoro-2-methylaniline

470 g of 5-bromo-4-fluoro-2-methylaniline (2.30 mol, 1.0 eq), 667 g of 2-bromocyclopropyl ketone (3.68 mol, 1.6 eq), organic solvent were added to the reaction flask. And alkali reagent, organic reagent is 3L toluene, alkali reagent is 623gDiisopropylamine ethylamine (4.83 mol, 2.1 eq), heated to 110 C for 12 hours, TLC detection showed the reaction was completed (PE / EA = 10/1, product Rf = 0.6, PE is petroleum ether, EA is Ethyl acetate). After the reaction: the mixture was cooled to room temperature, 1.5 liters of water and 1.5 liters of ethyl acetate were added, and the organic phase was separated with saturated ammonium chloride solution (500 mL), saturated sodium hydrogen carbonate solution (500 mL), and brine (500 mL) Wash once, dry anhydrous sodium sulfate (60g), spin dry, use 2L petroleum ether / acetic acidEthyl ester = 15/1 mixed solvent is beaten to obtain a solid product486 g (1.70 mol) of 2-(5′-bromo-4′-fluoro-2′-methylphenyl)amino-1-cyclopropyl ketone in a yield of 75%.

The synthetic route of 627871-16-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Douchuang (Shanghai) Pharmaceutical Technology Co., Ltd.; Wang Lei; Xu Zhi; Wang Zongying; Chen Da; Fu Haixiang; Li Ming; Ai Youqing; (11 pag.)CN109608441; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

Related Products of 86845-27-4, These common heterocyclic compound, 86845-27-4, name is 5-Bromo-2-methylbenzotrifluoride, 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.

To a solution of 4-Bromo-1-methyl-2-trifluoromethyl-benzene (3.4 g, 14.2 mmol) in THF was added n-BuLi at -78 C. After the reaction mixture was stirred at -78 C. for 30 minutes, dry acetone was slowly added. The resulting content was maintained at -78 C. for 3 hours and slowly warmed up to RT overnight. The reaction mixture was then partitioned between ethyl acetate and water. The ethyl acetate layer was then washed with brine, dried over Na2SO4, filtered, and the solvent evaporated in vacuo to yield a crude oil. The crude solid was purified via flash chromatography (15% EtOAc in n-hexane) yielded the title compound as an oil (2.7 g, 86%).1H NMR (400 MHz, CDCl3) delta 7.73 (d, 1H), 7.53 (dd, 1H), 7.25 (d, 1H), 2.47 (q, 3H), 1.58 (s, 6H).

Statistics shows that 5-Bromo-2-methylbenzotrifluoride is playing an increasingly important role. we look forward to future research findings about 86845-27-4.

Reference:
Patent; BIGNAN, Gilles; Gaul, Micheal; Xu, Guozhang; Zhao, Bao-Ping; US2011/150864; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 112279-60-4, 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. 112279-60-4, name is 4-Bromo-2,5-difluoroaniline, This compound has unique chemical properties. The synthetic route is as follows.

A degassed solution of ethyl 3-(nonafluorobutane-l-sulfonyloxy)-furo[3,2- c]pyridine-2-carboxylate (500 mg, 1.02 mmol), 4-bromo-2,5-difluoroaniline (277 mg, 1.33 mmol), Pd2dba3 (47 mg, 0.05 mmol), Xantphos (59 mg, 0.10 mmol) and DBU (388 mul, 2.56 mmol) in toluene (2.0 ml) was subjected to microwave irradiation at 15O0C for 10 minutes. The reaction mixture was concentrated and the resultant residue absorbed onto HM-N before being purified by flash chromatography (Si-SPE, cyclohexane: ethyl acetate, gradient 100:0 to 0: 100) to afford the title compound as a white solid (231 mg, 57%). LCMS (method B): Rx = 3.22 min, M+H+ = 397/399.

The chemical industry reduces the impact on the environment during synthesis 4-Bromo-2,5-difluoroaniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; GENENTECH, INC.; WO2008/24725; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 80058-84-0, name is 4-Bromo-2,6-diisopropylaniline, molecular formula is C12H18BrN, 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. Recommanded Product: 4-Bromo-2,6-diisopropylaniline

138 ml (2.59 mol) of96percent sulfuric acid was added dropwise to a solution of 4-bromo-2,6-diisopropylaniline (as prepared above, purity ca. 90percent) in 2000 ml of95percent ethanol cooled to -1 ooc at such a rate to keep the reaction temperature below 7°C. After the addition was complete, the formed solution was stirred at roomtemperature for 1 h. Then, the reaction mixture was cooled in an ice-bath, and asolution of 103.1 g (1.49 mol) of sodium nitrite in 215 ml of water was addeddropwise over ca. 1 h. The formed solution was stirred at the same temperature for30 min. Further on, the cooling bath was removed, and 18 g of copper powder was added. Upon completion of the rapid evolution of nitrogen additional portions (ca. 5g each, ca. 70 gin total) of copper powder were added with 10 min intervals untilgas evolution ceased completely. The reaction mixture was stirred at roomtemperature overnight, then filtered through glass frit (G3), diluted with two-foldvolume of water, and crude product was extracted with 4 x 200 ml of dichloromethane. The combined extract was dried over K2C03, evaporated todryness, and then distilled in vacuum (b.p. up to 120°C/5 mm Hg) to give ayellowish liquid. This product was additionally purified by flash-chromatography onsilica gel 60 ( 40-63 )lm; eluent: hexane) and distilled once again (b.p. 85-99°C/5mm Hg) to give 120.0 g (52percent) of 1-bromo-3,5-diisopropylbenzene as a colorless liquid.1H NMR (CDCh): b 7.19 (d, J = 1.2 Hz, 2H), 6.99 (br.t, 1H), 2.86 (sept, J = 6.9 Hz,2H), 1.24 (d, J= 6.9 Hz, 12H). 13CeH} NMR (CDCh): b 151.04, 126.85, 123.70,122.34, 34.06, 23.87

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 80058-84-0, its application will become more common.

Reference:
Patent; BOREALIS AG; AJELLAL, Noureddine; RESCONI, Luigi; IZMER, Vyatcheslav V.; KONONOVICH, Dmitry S.; OSKOBOYNIKOV, Alexander Z.; VIRKKUNEN, Ville; (133 pag.)WO2018/91684; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Application of 1435-53-6, 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. 1435-53-6, name is 2,4-Dibromo-1-fluorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

3-fluorophenol (0.333 mL, 3.68 mmol) and KOH (206 mg, 3.68 mmol) were stirred at 50 C for 30 mm before the addition of 2,4-dibromo-1-fluorobenzene (934 mg, 3.68 mmol) and Cu powder (234 mg, 3.68 mmol). The reaction mixture was heated to 150 C for 4 hrs and then shaken at 100 C overnight. Crudematerial was purified by FC on silica gel (eluent: cyclohexane), affording a mixture ?l:l of 2-bromo-1-fluoro-4-(3-fluorophenoxy)benzene and 4-bromo-1-fluoro-2-(3-fluorophenoxy)benzene (p13, 280 mg,y=26%).1H NMR (CHLOROFORM-d): 6 ppm 7.29 – 7.35 (m, 1 H) 7.21 – 7.27 (m, 1 H) 7.07 – 7.17 (m, 1 H) 6.96 -7.01 (m, 1 H) 6.81 – 6.89 (m, 1 H) 6.75 – 6.80 (m, 1 H) 6.67 – 6.74 (m, 1 H)

The chemical industry reduces the impact on the environment during synthesis 2,4-Dibromo-1-fluorobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SHIRE INTERNATIONAL GMBH; CREMONESI, Susanna; LUKER, Tim; SEMERARO, Teresa; MICHELI, Fabrizio; (257 pag.)WO2016/42452; (2016); 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. 54879-20-8, name is 2-Bromo-3-methylaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 2-Bromo-3-methylaniline

2-Bromo-3-methyl-phenylamine (1.06 g; CAS 54879-20-8), Boc2O (3.73 g) and DMAP (69 mg) in 50 ml THF were refluxed 2 hrs. The reaction mixture was concentrated, followed by an acidic extraction. The combined organic phases were dried over magnesium sulfate and evaporated. The crude product was taken in 50 ml methanol and K2CO3 (2.36 g) was added. The suspension was heated to reflux 2 h, and at rt for 18 h, evaporated and extracted with 0.5M HCl/AcOEt. The organic layers were dried over magnesium sulfate and chromatographed (silica gel; AcOEt/heptane, 1/9) to deliver a yellow oil (1.38 g). MS: 285/287 (M+H+)+.

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; Boehringer, Markus; Zbinden, Katrin Groebke; Haap, Wolfgang; Panday, Narendra; Ricklin, Fabienne; Stahl, Martin; Schmitz, Petra; US2007/112012; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Reference of 7617-93-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 7617-93-8 name is 2-Bromo-1,4-bis(trifluoromethyl)benzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Reference Production Example 50; To 13 ml of N,N-dimethylformamide was added 2 g of 1-bromo-2,5-bis(trifluoromethyl)benzene, 5.34 g of cesium carbonate, 0.24 g of tetrakis (triphenylphosphinepalladium) and 1.12 g of 4-pyridineboronic acid, and the mixture was stirred at 90C for 13 hours. Thereafter, the resultant reaction mixture was poured into a saturated ammonium chloride aqueous solution, and the mixture was extracted with ethyl acetate three times. The organic layers obtained by extraction were combined and washed with saturated saline, dried over anhydrous magnesium sulfate, then, concentrated. The resultant residue was subjected to silica gel column chromatography to obtain 1.6 g of 4-(2,5-bistrifluoromethylphenyl)pyridine. [Show Image] 1H-NMR:7.28(d,2H),7.59(s,1H),7.82(d,1H),7.94(d,1H),8.70-8.72 (m,2H)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Bromo-1,4-bis(trifluoromethyl)benzene, and friends who are interested can also refer to it.

Reference:
Patent; Sumitomo Chemical Company, Limited; EP2332936; (2011); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Adding a certain compound to certain chemical reactions, such as: 327-52-6, name is 1-Bromo-2,4,5-trifluorobenzene, 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 327-52-6, Quality Control of 1-Bromo-2,4,5-trifluorobenzene

To magnesium spalls in a reaction flask, under an atmosphere of nitrogen, was added 50 ml tetrahydrofuran and 0.02 g iodine as an initiator. A solution of 9g 1-bromo-2,4,5-trifluorobenzene in 150ml tetrahydrofuran was added dropwise into the reaction system. The reaction was stirred at 25 C for 3h to obtain a solution of 0.21 mol/L (2, 4, 5-trifluorophenyl)-magnesium bromide.

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-2,4,5-trifluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Zhejiang Jiuzhou Pharmaceutical Co., Ltd.; GAO, Hongjun; LI, Min; EP2551259; (2013); A1;,
Bromide – Wikipedia,
bromide – Wiktionary