Tag: M.W=300-400

Application of 344-03-6, 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. 344-03-6, name is 1,4-Dibromotetrafluorobenzene, This compound has unique chemical properties. The synthetic route is as follows.

(A) Preparation of starting materials Synthesis of dimethylaminomethyl p-bromotetrafluorobenzene 10 g (32.5 mmoles) of 1,4-dibromotetrafluorobenzene are dissolved under argon in 100 ml of ether and 100 ml of tetrahydrofuran. The solution is cooled to -78¡ã C. and 21 ml of a 1.6 molar solution of butyllithium in hexane are added. After 15 minutes, 6.08 g (65 mmoles) of N,N-dimethylmethyleneimmonium chloride are added and the mixture is warmed to room temperature. After 11/2 hours the mixture is poured into water and extracted with ether. The ethereal extract is dried over MgSO4. The solvent is distilled off, affording as residue a white solid which is distilled at 100¡ã C. under a high vacuum. Yield: 7.8 g (84percent) of a colourless product which is solid at room temperature.

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

Reference:
Patent; Ciba-Geigy Corporation; US4590287; (1986); A;,
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Application of 955959-84-9,Some common heterocyclic compound, 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan, molecular formula is C18H11BrO, 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 the 250 mE rounded-bottom flask, the compound Al (1.80 g, 10.64 mmol), the compound F2 (3.78 g, 11.70 mmol), tris(dibenzylideneacetone) dipalladium(0) (0.15 g, 0.16 mmol), (¡À)-2,2?-bis(diphenylphosphino)-l , 1 ?-binaphthalene(I3INAP) (0.20 g, 0.32 mmol) and sodium tertbutoxide(l.43 g, 14.89 mmol) were dissolved in toluene (100 mE) and stirred in the bath of the temperature of 100 C. for 24 hrs. After the completion of the reaction, toluene was removed, and the resultant was extracted and distilled under the reduced pressure using dichioromethane and water. After the silica gel colunm, the solvent was distilled under the reduced pressure such that the compound F3 was obtained. (3.05 g, 7.41 mmol)

The synthetic route of 955959-84-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LG DISPLAY CO., LTD.; LEE, Seung-Jae; BIN, Jong-Kwan; SEO, Bo-Min; CHOI, Hye-Ock; (62 pag.)US2018/97184; (2018); A1;,
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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 3975-77-7 as follows. Recommanded Product: 3975-77-7

General. 1H NMR studies revealed that?supermesityl bromide? (mes*Br, S1)S7 and n-BuLi coexist in t-BuOMeover more than 18 h at room temperature, while this solvent is very slowlydeprotonated by n-BuLi with formation of isobutene. Similarly, t-BuLideprotonates t-BuOMe, leaving S1intact.When prepared from S1 withn-BuLi, mes*Li (S2)is not stable in a THF solution at ambient temperature. However, its stabilityis greatly enhanced on dilution of the THF with pentane. Moreover, a portion ofS2 will crystallize from pentane/THF(4:1)S8 and may be washedwith dry petroleum ether if pure mes*Li is required.In Et2O atroom temperature, the formation of mes*Li(S2) from S1and n-BuLiwas complete within 10 min; therefore,the traditional long reaction periods of this Br/Li interchange reaction in thesolvent Et2O can be considerably shortened, and the presence of apromoter (such as TMEDA) is unnecessary.This Et2O solution containing S2 and 1-bromobutane was stable for several hours at ambienttemperature and for at least 18 hours under argon gas in a refrigerator. Although S2in Et2O was protonated very slowly by N,N-diisopropylamine atroom temperature, proton transfer fromcyclohexylamine (pKa =41.6) to S2 was fast andquantitative. Procedure. A dry NMR tube (5 mm) was charged with mes*BrS7 (S1,80 mg, 0.24 mmol), pentane (0.40 mL), and anhydrous THF (0.10 mL), then cooled to -70 C during the addition of n-BuLi (0.37 mmol) in hexanes (0.14 mL)and for further 60 min. The colorless precipitate of S2 was washed with pentane (2 ) and then dissolved in anhydrous Et2O(0.50 mL), showing dH = 7.01 ppm for 3-/5-H of S2. The addition of cyclohexylamine (0.027 mL, 0.24 mmol) at -70 C converted S2 completely into 1,3,5-tri-tert-butylbenzene(dH = 7.31 ppm), which was isolated afterquenching with solid CO2 andaqueous workup (no acid S3) as apure, colorless powder (35 mg, 58%). This indicates that pKa> 41.6 for S2. A similar run with N,N-diisopropylamine(ca. 2 equiv, pKa = 34.4)in place of cyclohexylamine disclosed a very slow proton transfer at room temperature (ca. 30% in 10 min).

According to the analysis of related databases, 3975-77-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Knorr, Rudolf; Rossmann, Eva C.; Knittl, Monika; Boehrer, Petra; Tetrahedron; vol. 70; 34; (2014); p. 5332 – 5338;,
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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. 18869-30-2, name is (E)-1,2-Bis(4-bromophenyl)ethene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 18869-30-2

EXAMPLE 3 Ethyl 4-bromostilbene-4′-acrylate. 25.8 g (0.1 mol) of 4,4′-dibromostilbene, 10 g (0.1 mol) of ethyl acrylate, 18.5 g (0.1 mol) of tri-n-butylamine, 0.224 g (0.001 mol) of palladium acetate and 0.6 g (0.002 mol) of tri-o-tolylphosphine are added under argon to 50 ml of p-xylene. The reaction mixture is stirred at 90 C. for 4 hours. Working up gives 2 g (6% of theory) of ethyl 4-bromostilbene-4′-acrylate. Melting point 166.9 C.

The synthetic route of 18869-30-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ciba-Geigy Corporation; US4918215; (1990); A;,
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72678-19-4, 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. 72678-19-4, name is 2,6-Dibromo-4-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below.

A mixture of 2,6-dibromo-4-(trifluoromethyl)aniline [72678-19-4] (5.13 g, 16.1 mmol), triemthylboroxine [823-96-1] (5 mL, 35.3 mmol), Pd(PPh3)4 (1.11 g, 1.00 mmol) and K2C03 (sat., aq., 74 mL) in DME (74 mL) was stirred at 150 C for 2 h. The mixture was concentrated in vacuo and the residue was taken up in water and DCM. The organic phase was separated, dried (MgS04), filtered and evaporated in vacuo. The crude mixture was purified by flash column chromatography (silica, heptane/EtOAc, gradient from 100:0 to 50:50) to afford 1-131 (1.86 mg, 61%) as a brown oil.

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; JANSSEN PHARMACEUTICA NV; BARTOLOME-NEBREDA, Jose Manuel; TRABANCO-SUAREZ, Andres, Avelino; TRESADERN, Gary John; MARTINEZ LAMENCA, Carolina; LEENAERTS, Joseph Elisabeth; OEHLRICH, Daniel; BUIJNSTERS, Peter Jacobus Johannes Antonius; VELTER, Adriana, Ingrid; VAN ROOSBROECK, Yves, Emiel, Maria; (171 pag.)WO2019/243535; (2019); A1;,
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Adding some certain compound to certain chemical reactions, such as: 3344-70-5, name is 1,12-Dibromododecane, 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 3344-70-5. 3344-70-5

Take 1.19 g of compound 6,3.15 g of 1,2-dibromododecane, 0.15 g of tetrabutylammonium bromide, 0.36 g of hydroxidePotassium, 14 ml of water and 22 ml of methylene chloride, and the mixture was stirred at room temperature for 24 hours under a nitrogen atmosphere. The organic layer was separated with 15 mlLiter of methylene chloride. The organic layer was collected and the organic layer was washed with 15 ml of saturated brine,Layer, dried over anhydrous sodium sulfate. After removal of water, the solvent was removed by rotary distillation under reduced pressure. The resulting crude product was washed with 200-300 mesh silica gel column(Eluent: petroleum ether / ethyl acetate, 100: 1 by volume) to give compound 7, 1.20 g of an off-white solid, yield75.60percent.

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 1,12-Dibromododecane.

Reference:
Patent; Guilin University of Technology; Kong, Xiangfei; Xia, Liting; Yao, Wei; Gong, Hongkang; Wang, Guixia; (8 pag.)CN106588941; (2017); A;,
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88223-35-2, 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. 88223-35-2, name is 2-Bromo-9,9-dibutyl-9H-fluorene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In a 250 mL round bottom flask was placed 7 (14.2 g, 40 mmol). The flask was evacuated under vacuum and flushed with nitrogen three times. THF (150 mL) was then added. The mixture was cooled to -78 C and n-BuLi (19.2 mL, 48 mmol) was slowly added. After the mixture was stirred for 5 h at -78 C, trimethyl borate (5.6 mL, 48 mmol) was injected. After 2 h, the mixture was slowly warmed to room temperature. HCl (3 M, 150 mL) solution was added and the mixture was stirred for another 3 h. The mixture was extracted with DCM three times. The combined organic layers were washed with water, dried over anhydrous sodium sulfate. The product was then dried under high vacuum. The crude product was condensed and purified on a silica-gel column using a mixture of DCM and acetone (5:1 by volume) as eluent. A white solid 4d (5.83 g, 45.3% yield) was obtained; m.p. 145-148 C. 1H NMR (300 MHz, d6-DMSO): delta (ppm): 7.98 (s, 2H), 7.83 (s, 1H), 7.74-7.82 (m, 3H), 7.43-7.45 (m, 1H), 7.31-7.34 (m, 2H), 1.95-1.99 (m, 4H), 0.98-1.06 (m, 4H), 0.61 (t, 6H, J = 7.5 Hz), 0.46-0.50 (m, 4H).

The synthetic route of 2-Bromo-9,9-dibutyl-9H-fluorene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhu, Tianhao; He, Guangke; Chang, Jin; Zhao, Dongdong; Zhu, Xiaolin; Zhu, Hongjun; Dyes and Pigments; vol. 95; 3; (2012); p. 679 – 688;,
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626-39-1, Adding a certain compound to certain chemical reactions, such as: 626-39-1, name is 1,3,5-Tribromobenzene, 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 626-39-1.

Carbazole (6.6 g, 39.7mmol), 1,3,5-tribromobenzene (5 g, 15.9mmol), cuprous iodide (0.3 g,1.6 mmol), potassium phosphate (13.7 g, 64.5 mmol) and trans-1,2-cyclohexanediamine(1.6 g, 15.9 mmol) were dissolved in 200 mL of 1,4-dioxane. After the mixed solution wasstirred in a nitrogen atmosphere for 19 h at 110C, the reaction mixture was cooled to roomtemperature. The mixture extracted with dichloromethane (80 mL ¡Á 3 times) and driedover anhydrous MgSO4. The crude product was subjected to flash column chromatography(dichloromethane: n-hexane = 1: 4) to give compound (1) (6.3 g, 79%). 1H NMR (CDCl3,300MHz); delta = 7.68 (d, -CH-), 7.5 (d, -CH-), 7.45 (d, -CH-), 7.35 (m-CH-), 7.29(t, -CH3),7.18(m, -CH-).

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, 1,3,5-Tribromobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Yun, Seong-Jae; Seo, Minhye; Lee, Sungkoo; Molecular Crystals and Liquid Crystals; vol. 662; 1; (2018); p. 82 – 90;,
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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. 955959-84-9, name is 4-(4-Bromophenyl)dibenzo[b,d]furan belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 955959-84-9

In the argon atmosphere, weighing intermediate respectively (1-1) 3.2g (10.0mmol), intermediate (A-2-1) 5.8g (10.0mmol), Pd2(dba)30.14g (0.15mmol), P (tBu)3HBF40.087g (0.3mmol), tertiary butyl alcohol sodium 1.9g (20.0mmol), adding anhydrous xylene 50 ml, heating reflux for 8 hours.After the reaction, the reaction mixture is cooled to 50 ¡ãC, filtered through diatomaceous earth/silica gel, concentrated filtrate. The obtained concentrated residue after being refined with silica gel column chromatography, using toluene recrystallization, get 2.9g of the white crystal (yield 35percent).

The synthetic route of 955959-84-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; Jiateng, Pengxi; Sounei, Shenhao; Zhou, Qiaozhenghe; Tengshan, Gaoguang; (107 pag.)CN105431417; (2016); A;,
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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. 10016-52-1, name is 2,8-Dibromodibenzo[b,d]furan belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 10016-52-1

Dibromodibenzo [b, d] furan (1.0 g, 3.07 mmol, 1.0 eq) was dissolved in tetrahydrofuran (35 ml) followed by the addition of Tetrahydrofuran To a 25 ml flaskThe mixture was gradually added at 45 and stirred. After completion of the reaction, the reaction mixture was distilled under reduced pressure to remove the solvent. The solvent was distilled off (100 ml X 3), and the filtrate was dried over MgSO 4, filtered, and dried to obtain dibenzo [b, d] furan-2,8-diylbis ) Phenyl) methanol (1.7 g). The solution was dissolved in 35 ml of methanol and 35 ml of hydrogen chloride, followed by heating and stirring at 80 C for 2 hours. After the reaction was completed, the solvent was distilled off to remove the solvent, and then a small amount of distilled water was added thereto. After the work-up, water was removed with MgSO 4 and filtered to obtain G-4 (1.3 g, yield 63.17%

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

Reference:
Patent; Korea Jiao Tong University Academic Cooperation; Lee, Ji Hun; Choe, Sung Hyun; Yun, Poo Yong; Yun, Moo Sang; (25 pag.)KR101638767; (2016); B1;,
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