Bromides-buliding-blocks

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. 203302-95-8, name is 4-Bromo-3,5-difluoroaniline, A new synthetic method of this compound is introduced below., Quality Control of 4-Bromo-3,5-difluoroaniline

4-bromo-3.5-difluoro-aniline 1 g (4.81 mmol) and m-methoxyphenylboronic acid 730 mg (4.81 mmol. 1 eq)Potassium carbonate (4.82 g 24.88 mmol 6 eq) [1,1′-bis(diphenylphosphino)ferrocene]palladium dichloride (425.35 mg481 mmol 6 eq) was placed in a 100 ml two-necked flask, and 30 ml (dioxane: water = 3:1) was injected with nitrogen to protect the solution, and 80 was allowed to react for 3.5 h. After the TLC monitoring reaction is completed, the post-treatment distillation is carried out under reduced pressure to about 10 ml, and the solution is poured into a separating funnel, extracted with dichloromethane for 2-3 times, dried over anhydrous Na 2 SO 4 , filtered, and evaporated to dryness to give a black oily drop. Separated and purified by petroleum ether: ethyl acetate = 6:1 silica gel column chromatography to obtain a pale yellow oily liquid about 690 mg, yield 61%.

The synthetic route of 203302-95-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan University; Zhao Yinglan; Luo Youfu; Wei Yuquan; (63 pag.)CN108467370; (2018); A;,
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Synthetic Route of 17247-58-4, 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. 17247-58-4, name is (Bromomethyl)cyclobutane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of KOtBu (28 g, 249.5 mmol) in THF (180mL) was slowly added drop wise to a stirred solution ofdiphenylimine protected ethyl glycinate (60 g, 224.4 mmol),cyclobutyl methyl bromide (33.5 g, 224.8 mmol) in THF(180 mL) at 50 C within 15 min and the mixture was stirredat 60 C for 6 h. After completion of reaction (monitored byTLC), reaction temperature allowed to cool to 10 C and 2NHCl (100 mL) was added to reaction mixture by maintainingthe temperature below 15 C. After being stirred at rt for 7 h, DCM (400 mL) was added and the pH adjusted to above 12.By separating both the layers aqueous layer was re-extractedusing DCM (250 mL). The combined organic layers werewashed with brine (240 mL), dried over sodium sulfate, filteredthrough a plug of cotton and concentrated under reducedpressure to obtain the desired amino ester (51.8 g,85%) as colorless oil. 1H NMR (400M Hz, CDCl3) delta (ppm):1.25 (t, 3H, J = 6.8 Hz), 1.65-2.14 (m, 8H), 2.42-2.48 (m,1H), 3.72 (q, 2H, J = 6.8 Hz), 3.87-3.93 (m, 1H); MS m/z:172.2 ([M+H]+); IR (KBr) (upsilonmax, Cm-1): 1731.5 (C=O),3314.9 (-NH2), 3379.7 (-NH2).

The synthetic route of (Bromomethyl)cyclobutane has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yerrabelly, Jayaprakash Rao; Rebelli, Pradeep; Yalamanchili, Bharathi Kumari; Ghojala, Venkat Reddy; Letters in Organic Chemistry; vol. 13; 5; (2016); p. 352 – 358;,
Bromide – Wikipedia,
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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. 4263-52-9, name is Sodium 2-bromoethanesulphonate, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 4263-52-9

A mixture of (E)-1,2-di(4-pyridyl)ethylene (91 mg, 0.5 mmol) and sodium 2-bromoethanesulfonate (317 mg, 1.5 mmol) (Aldrich) in abs. EtOH (3 mL) was refluxed with stirring for 50 h. The insoluble substance was filtered, washed with benzene, MeOH, and acetone, and re-crystallized from water-EtOH (2.8:1 (v/v), 2.7 mL) to yield 128 mg (64%) of (E)-3a as a pinkish powder.

According to the analysis of related databases, 4263-52-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Vedernikov, Artem I.; Lobova, Natalia A.; Kuz’mina, Lyudmila G.; Howard, Judith A.K.; Strelenko, Yuri A.; Alfimov, Michael V.; Gromov, Sergey P.; Journal of Molecular Structure; vol. 989; 1-3; (2011); p. 114 – 121;,
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7745-91-7, name is 3-Bromo-4-methylaniline, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. category: bromides-buliding-blocks

The solution of 4-methoxy-1,3-benzenedichloride (6)(0.93 g, 4.0 mmol) in anhydrous THF (15 mL) was added to3-bromine-4-methylaniline (1.48 g, 8.0 mmol). This solutionwas stirred rapidly at room temperature for about 1 hand then pyridine (1 mL) was added. The solution wasrefluxed for 4-8 h. The residue was recrystallized frommethanol-water to terminal compound 1a (1.81 g, yield85.2%). The other compounds (1b-1i) were prepared with thesimilar method of preparing compound 1a. White solid (The residue was recrystallized by 50%ethanol.); Yield = 85.2%; Rf: 0.38; m.p.: 157.2-158.4 C;IR (KBr) upsilonmax 3340.21, 2971.89, 1665.12, 1601.07,1447.33, 1267.97, 982.92, 758.72 cm-1; 1H-NMR(400 MHz, CDCl3, TMS): delta = 10.06 (s, 2H, 2¡Á -CONH-),8.72 (s, 1H, Ar-2-H), 8.62 (d, J = 6.8 Hz, 1H, Ar-6-H), 8.42(d, J = 7.2 Hz, 1H, Ar-5-H), 8.15 (s, 2H, Ar-2?,2?-H), 7.86(d, J = 4.8 Hz, 2H, Ar-6?, 6?-H), 7.49 (d, J = 7.8 Hz, 2H,Ar-5?, 5?-H), 3.78 (s, 3H, Ar-4-OCH3), 1.43 (s, 6H, Ar-4?,4?-CH3); 13C-NMR (101 MHz, CDCl3): delta = 164.49 (C, C= O), 163.42 (C, C = O), 142.57 (C, Ar-4-C), 141.97 (C,Ar-1?-C), 139.68 (C, Ar-1?-C), 133.63 (C, Ar-1-C), 133.13(C, Ar-3-C), 132.29 (C, Ar-3?-C), 131.26 (C, Ar-3?-C),130.28 (CH, Ar-2-C), 128.92 (CH, Ar-6-C), 127.83 (CH,Ar-5-C), 126.23 (CH, Ar-2?-C), 124.63 (CH, Ar-2?-C),122.65 (CH, Ar-5?-C), 121.31 (CH, Ar-5?-C), 118.91 (CH,Ar-6?-C), 117.79 (CH, Ar-6?-C), 116.46 (C, Ar-4?-C), 115.36 (C, Ar-4?-C), 63.49 (O-CH3, Ar-4-O-CH3), 14.76(2¡Á CH3, Ar-4?,4?-CH3); MS (m/z): 532.9820 [M + H]+.

The synthetic route of 7745-91-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Guangling; Wang, Chaoqing; Zhang, Zhihao; Liu, Xiujie; Medicinal Chemistry Research; vol. 28; 9; (2019); p. 1413 – 1424;,
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Application of 100189-84-2, A common heterocyclic compound, 100189-84-2, name is 2,5-Dibromo-1,3-dimethylbenzene, molecular formula is C8H8Br2, 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.

In a 25 mL Schlenk tube, 200 mg of 2,5-dihexyldioctyl-3,6-bisthiophenepyrrole [3,4-c]-pyrrole-1,4-dione was added according to a 2:1 molar ratio. Monomer 1), 35.2 mg of 2,6-dimethyl-1,4-dibromobenzene (monomer 4), sequentially added 200 mg of cesium carbonate, 8 mg of pivalic acid, 4 mg of Pd2(dba)3 catalyst, 3.3 mg of P ( o-MeOPh) 3 ligand. The moles of the catalyst Pd2(dba)3, the ligand P(o-MeOPh)3, the promoter pivalic acid PivOH, and the base Cs2CO3 were 1.5%, 3%, 30%, and 200%, respectively, of the monomer 1. In 6 mL of anhydrous toluene, the mixture was stirred under an inert atmosphere and heated to 120 C for 46 h. The obtained crude product was separated by silica gel column chromatography, and different conjugate length oligomers were collected, and the obtained solid product was vacuum dried under a rotary evaporator to obtain three conjugated oligomers of increasing degree of polymerization. , O8 and O9.The yields of O7, O8 and O9 are 35%, 30% and 25%, respectively.

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; Jiangxi University of Science and Technology; Liu Shiyong; Shen Zhaoqi; Liu Hui; Liu Lilin; Wen Herui; (20 pag.)CN108752367; (2018); A;,
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Related Products of 39478-78-9, 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. 39478-78-9, name is 5-Bromo-2-methylaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Reference Example 355-Cyclopropyl-2-methylanilineAt room temperature, to a suspension of 5-bromo-2-methylaniline (372 mg), cyclopropylboronic acid monohydrate (270 mg), tricyclohexylphosphine (56.0 mg), and potassium phosphate (1.49 g) in toluene (8.0 mL)-water (0.4 mL) was added palladium (II) acetate (22.4 mg), and the mixture was stirred under an argon gas atmosphere at 100 C. for 6 hours. To the reaction mixture were added water and ethyl acetate, and the organic layer was separated. The aqueous layer was extracted with ethyl acetate and the organic layer was combined. The layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The obtained crude product was purified by silica gel column chromatography (eluting solvent: hexane-ethyl acetate) to obtain the title compound (256 mg).

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, 5-Bromo-2-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; KISSEI PHARMACEUTICAL CO., LTD.; US2012/122931; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 25017-13-4, name is 1-(2-Bromoethyl)-3-fluorobenzene, 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. SDS of cas: 25017-13-4

3-Fluorophenethyl Cyanide (24). 3-Fluorophenethyl bromide (23, 1.00 g, 12.3 mmol) was diluted in dry DMF (25 mL). Sodium cyanide (1.06 g, 61.6 mmol) was added in one portion, and the mixture was heated to 60 C. under argon for 16 h. The mixture was cooled and concentrated, and the residue was partitioned between EtOAc and H2O (50 mL each). The layers were separated, and the aqueous phase was extracted with EtOAc (2¡Á20 mL). The organic layers were washed with H2O and sat. aq. NaCl (50 mL each), dried over anhydrous sodium sulfate, and concentrated. The resulting oil was purified by flash column chromatography (SiO2), eluting with a gradient of 5% EtOAc in hexanes to 30% EtOAc in hexanes to yield the desired product as a colorless oil (0.638 g, 87%). 1H-NMR (500 MHz; CDCl3): delta 7.31 (td, J=7.9, 6.0 Hz, 1 H), 7.03-6.93 (m, 3 H), 2.96 (t, J=7.4 Hz, 2 H), 2.63 (t, J=7.4 Hz, 2 H).

The synthetic route of 1-(2-Bromoethyl)-3-fluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Northwestern University; Silverman, Richard B.; Cinelli, Maris A.; US9212144; (2015); B2;,
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Adding a certain compound to certain chemical reactions, such as: 1647-23-0, name is 1-Bromo-3,3-dimethylbutane, 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 1647-23-0, Recommanded Product: 1-Bromo-3,3-dimethylbutane

1-(2-Chloro-phenyl)-4,4-dimethyl-pentan-1-one 14.1 g (580 mmole) Magnesium turnings were placed in a 1 l-roundbottom flask equipped with a dropping funnel and a reflux condenser, and 60 ml of THF were added. The magnesium was etched slightly with a few crystals of iodine and then 2 g of 1-bromo-3,3-dimethyl-butane were added and the mixture was heated locally. After the start of the Grignard-formation the rest of the 1-bromo-3,3-dimethyl-butane in 350 ml of THF (88.1 g in total, 533 mmole) were added within a period of 20 min. The mixture was refluxed for 1.5 h and then cooled to room temperature. In a separate 2 l-roundbottom flask 63.9 g (464 mmole) of 2-chloro-benzonitrile and 141 mg (0.16 mole %) copper(I)iodide were dissolved in 265 ml of THF. The Grignard-solution was added dropwise over a period of 30 min and the reaction mixture was refluxed for 3 h. After standing overnight at room temperature, a mixture of 190 ml water and 127 ml concentrated hydrochloric acid were added very carefully, causing a strongly exothermic reaction. The mixture was stirred at 50 C. for 1 h and the layers were separated. The aqueous layer was extracted twice with 150 ml of toluene each. The combined organic layers were washed twice with 2 M sulphuric acid, once with a saturated sodium bicarbonate solution and once with a saturated sodium chloride solution. After drying over magnesium sulphate the solvent was evaporated in vacuo to yield 103.8 g (quant.) of the desired phenone as slightly brown oil. 1H-NMR (400 MHz, CDCl3): delta=7.41-7.26 (m, 4H, aromatic), 2.87 (m, 2H, COCH2), 1.59 (m, 2H, CH2-t-Bu), 0.90 (s, 9H, t-Bu) ppm.

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

Reference:
Patent; Lammus Novolen Technology GmbH; US8299287; (2012); B2;,
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. 153505-37-4, name is 4-Bromo-5-fluorobenzene-1,2-diamine, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 153505-37-4

The compound was synthesized starting from (S)-4-phenyloxazolidin-2-one (1 equiv., 0.328 g, 2 mmol), 4-bromo-5-fluorobenzene-1,2-diamine (1 equiv., 0.412 g, 2 mmol), copper(I) iodide (0.1 equiv., 0.040 g, 0.2 mmol), cesium fluoride (2 equiv., 0.608 g, 4 mmol), cyclohexane-1,2-diamine (0.1 equiv., 0.024 mL, 0.2 mmol). The dried solids were given together in a reaction flask and the flask was purged with argon. A solution of cyclohexane-1,2-diamine in 4 mL dioxane was added to the flask. The reaction was stirred at 95 C. for 48 hours, before the reaction was cooled down to 45 C. and filtered through a pad of CELITE. The pad was washed with warm dichloromethane and the solution was concentrated under reduced pressure. The intermediate product was purified via FPLC using a chloroform-methanol gradient (0?10%, product elutes at about 5%).Yield: 0.078 g (13.6%)

According to the analysis of related databases, 153505-37-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PROBIODRUG AG; US2011/92501; (2011); A1;,
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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