Tag: M.W=200-300

These common heterocyclic compound, 454-79-5, name is 2-Bromo-5-(trifluoromethyl)aniline, 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. Recommanded Product: 2-Bromo-5-(trifluoromethyl)aniline

2.40 g of 2-bromo-5-trifluoromethyl-aniline and1.21 g of potassium ethylxanthate were dissolved in 35 ml of DMF solution, reacted under refluxing at 120 degree centigrade, and then reacted overnight under stirring at room temperature. TLC detection was performed and it was confirmed that raw materials no longer decreased, and the reaction was completed. The product was washed with 25 ml of dilute hydrochloric acid solution, organic layer was extracted, combined and dried, and column chromatography was carried out to obtain 1.70 g of an oily liquid (yield 72%). Mass spectrum MS of the compound: [M+H] 235.2.

The synthetic route of 2-Bromo-5-(trifluoromethyl)aniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DRIVINGFORCE THERAPEUTICS Co., Ltd.; YANG, Yongliang; (20 pag.)US2018/29979; (2018); A1;,
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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. 4549-33-1, name is 1,9-Dibromononane, A new synthetic method of this compound is introduced below., Application In Synthesis of 1,9-Dibromononane

Under inert atmosphere, to a stirred solution of NaH (140 mg, 3.45 mmol) in 2 ml anhydrous DMF at 0C, it was added a solution of theophylline (378 mg, 2.098 mmol) in 10 ml anhydrous DMF. After 2 h at room temperature, 1,9-dibromononane (142 mu, 1.41 mmol) was slowly added to the reaction mixture. This mixture was stirred at room temperature overnight, and then solvent was completely removed. The crude was chromatographically purified over Si02 using gradient mixtures of AcOEt/MeOH as the eluant, yielding 0.108 g (32 %) of the desired product B. NMR (400 MHz, DMSO-d6): delta 8.07 (s, 2 H), 4.22 (t, J=7.0 Hz, 1 H), 3.42 (s, 6 H), 3.22 (s, 6 H), 1.69 – 1.83 (m, 4 H), 1.24 (br. s., 10 H) ppm. MS (ESI (+)): m/z = 507.2 [M+Na]+ MS (ESI (-): m/z = 483.0 [M-H]”

The synthetic route of 4549-33-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITAT DE VALENCIA; INSTITUT QUIMIC DE SARRIA CETS FUNDACIO PRIVADA; INSTITUT UNIV. DE CIENCIA I TECNOLOGIA, S.A.; ARTERO ALLEPUZ, Ruben; CASTELLS BOLIART, Josep; BORRELL BILBAO, Jose Ignacio; LLAMUSI TROISI, Beatriz; BARGIELA SCHOeNBRUNN, Ariadna; KONIECZNY, Piotr; PASCUAL GILABERT, Marta; TEIXIDO CLOSA, Jordi; ESTRADA TEJEDOR, Roger; LOPEZ GONZALEZ, Alejandro; (68 pag.)WO2016/75285; (2016); A1;,
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These common heterocyclic compound, 73918-56-6, name is 2-(4-Bromophenyl)ethanamine, 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. Product Details of 73918-56-6

To a pre-cooled 0 C. solution of 112 (2.0 g, 10 mmol) in THF (10 mL) was added (Boc)2O (2.2 g, 10 mmol) portionwise. The reaction mixture was stirred at room temperature over night. It was concentrated in vacuo to yield 113 (3 g, 100%) as a white solid which was used in the next step without further purification.

The synthetic route of 2-(4-Bromophenyl)ethanamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hydra Biosciences; US2007/219222; (2007); A1;,
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Related Products of 69272-50-0,Some common heterocyclic compound, 69272-50-0, name is 3,6-Dibromobenzene-1,2-diamine, molecular formula is C6H6Br2N2, 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.

1) Preparation of 5,8-dibromo-2,3-bis(phenyl)quinoxaline, the Chemical Equation Thereof is The detailed preparation procedure is as follows: 3,6-dibromo-o-phenylene diamine (1.0 g, 3.7 mmol) was added to a solution of compound benzil (0.39 g, 1.84 mmol) in acetic acid (20 mL) at 120?, then the mixture was mixed uniformly. After refluxed for 12 hours, the fluid reactant was poured into water, and neutralized with sodium bicarbonate until neutral, then extracted with chloroform and washed with saturated brine, dried over anhydrous sodium sulfate, then it was vacuum evaporated to remove the solvent, and the resulting crude product was purified by column chromatography to give a white solid, and then it was purified by recrystallization from chloroform/n-hexane to give a white solid powder. The test result is: MS (EI) m/z: 440(M+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,6-Dibromobenzene-1,2-diamine, its application will become more common.

Reference:
Patent; Ocean’s King Lighting Science & Technology Co., Ltd.; Zhou, Mingjie; Huang, Jie; Xu, Erjian; US8853348; (2014); B2;,
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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. 454-79-5, name is 2-Bromo-5-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., Application In Synthesis of 2-Bromo-5-(trifluoromethyl)aniline

Reference Example 94 Synthesis of 2-(2-methyl-6-trifluoromethyl-1H-indol-3-yl)acetic acid A mixture of 3-amino-4-bromobenzotrifluoride (1.2 g), levulinic acid (1.0 g), p-TsOH (0.1 g) and benzene (10 ml) was heated to reflux for 3 hours using a Dean Stark tube. The reaction mixture was concentrated under reduced pressure, and a mixture of palladium acetate (60 mg), tris(o-tolyl)phosphine (0.15 g), triethylamine (0.8 g) and DMF (2 ml) was stirred with the obtained residue in a sealed tube for 20 hours at 120 C. Water and ethyl acetate were added to the reaction mixture, the insoluble portion was filtered out with celite and extraction was performed with ethyl acetate, and then after combining the organic layer and drying over sodium sulfate, the product was concentrated under reduced pressure. Methanol (20 ml) and concentrated sulfuric acid (1 ml) were added to the obtained residue and the mixture was heated to reflux for 2 hours. Water was added to the reaction mixture, which was then extracted with dichloromethane, dried over sodium sulfate and concentrated under reduced pressure. 2-(2-methyl-6-trifluoromethyl-1H-indol-3-yl)acetic acid methyl ester was purified from the obtained residue by silica gel column chromatography using a mixed solvent of hexane and dichloromethane. A 2 N sodium hydroxide aqueous solution (1 ml) and methanol (1 ml) were added to the obtained 2-(2-methyl-6-trifluoromethyl-1H-indol-3-yl)acetic acid methyl ester, and the mixture was heated to reflux for one hour. Water was added to the reaction mixture, which was then rendered acidic with concentrated aqueous hydrochloric acid, extracted with ethyl acetate, dried over sodium sulfate and concentrated under reduced pressure, to obtain 79 mg of the title compound as a colorless powder (6% yield). The NMR data for the obtained compound were as follows. NMR: (300 MHz, DMSO-d6) delta: 2.38 (3H,s), 3.62 (2H,s), 7.23 (1H,dd), 7.5-7.7 (2H,m), 11.32 (1H,s), 12.0-12.4 (1H,m)

The synthetic route of 454-79-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Fujiwara, Shinya; Ozaki, Tomokazu; Kozono, Toshiro; Hattori, Kunihiro; Esaki, Toru; US2003/162724; (2003); A1;,
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Application of 15155-41-6, 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. 15155-41-6, name is 4,7-Dibromo-2,1,3-benzothiadiazole belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

4,7-Dibromo-2,1,3-benzothiadiazole (12.204 g, 42.5 mmol) was added to a 500 ml three-neck round bottom flask, dissolved in 400 ml of absolute ethanol, passed through a nitrogen atmosphere, and cooled to 0 C. NaBH4 (15.69 g, 425 mmol) was added portionwise to the solution. After the addition of NaBH4, the reaction mixture was transferred to room temperature overnight. The reaction solution was poured into a beaker, and the solid precipitated in the bottle was completely dissolved by adding 50 ml of water. The large amount of ethanol in the bottle was removed, extracted with dichloromethane and water, and the combined organic phases were washed with water, dried over anhydrous magnesium sulfate and filtered.The filtrate was distilled under reduced pressure to give a pale yellow solid (7.583 g, 28.74 mmol, 67.6%).That is, 3,6-dibromo-1,2-phenylenediamine, the structural formula is:

The synthetic route of 4,7-Dibromo-2,1,3-benzothiadiazole has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangxi Normal University; Liang Aihui; Zhou Wenjing; Xie Qi; Zhang Jiayu; Liu Zhiqian; Hu Sifan; (26 pag.)CN110204561; (2019); A;,
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Reference of 100189-84-2, 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. 100189-84-2, name is 2,5-Dibromo-1,3-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 2,5-dibromo-1,3-dimethylbenzene (2640 mg, 10 mmol, Oakwood Products, Inc. – 018507) in anhydrous acetonitrile (25 mL) was added palladium(U) acetate (112 mg, 0.5 mmol), acrylonitrile (531 mg, 10 mmol), tri(o-tolyl)phosphine (131 mg, 0.5 mmol) and triethylamine (4 mL, 30 mmol) then the mixture was purged with argon and heated at 110 C for 2 hours. The reaction mixture was filtered through Celite and the filter pad was washed with tetrahydrofuran (10 mL). The filtrate was evaporated then re-dissolved with ethyl acetate (50 mL). The solution was washed with water (50 mL). The water layer was back extracted with ethyl acetate (50 mL). The combined organics were washed with brine (30 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure to give a crude residue. This was subjected to silica gel chromatography (gradient from 0-20% ethyl acetate in iso-hexanes) to afford the crude product which was treated in sonic bath with hexane (10 mL) for 10 minutes. The product precipitated out of solution and was collected by filtration. The solids were washed with cold hexane to afford compound id. ?H NMR (400 MHz, CDC13) 67.25 (d,J= 16.6 Hz, 1H), 7.12 (s, 2H), 5.84 (d,J 16.6 Hz, 1H), 2.42 (s, 6H). LCMS (mlz) no MS signal, Tr = 2.78 mm (LCMS method 1).

The chemical industry reduces the impact on the environment during synthesis 2,5-Dibromo-1,3-dimethylbenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; GILEAD SCIENCES, INC.; JANSA, Petr; MACKMAN, Richard, L.; HU, Yunfeng, Eric; LANSDON, Eric; (81 pag.)WO2016/105534; (2016); A1;,
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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. 1435-52-5, name is 1,4-Dibromo-2-fluorobenzene, A new synthetic method of this compound is introduced below., Quality Control of 1,4-Dibromo-2-fluorobenzene

150ml three-necked flask, add 0.01 mol of 2,5-dibromofluorobenzene, 0.012 mol M1, 0.02 mol sodium carbonate and 10 ml ethylene glycol dimethyl ether, It was purged with nitrogen, heated to 190 ¡ã C, and stirred for 48 hours. Then cooled to room temperature and poured into a beaker.Add 50 ml of toluene and 50 ml of water and stir for 20 minutes. Filtration, the filtrate is steamed, passed through a silica gel column, Obtaining white intermediate 1a, The purity was 98.60percent, and the yield was 80.5percent.

The synthetic route of 1435-52-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangsu March Optoelectric Technology Co., Ltd.; Ye Zhonghua; Zhang Zhaochao; Li Chong; Zhang Xiaoqing; (57 pag.)CN109575057; (2019); A;,
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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. 502496-36-8, name is 3-Bromo-5-fluoro-2-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 502496-36-8

A suspension of 3-bromo-5-fluoro-2-methyl-aniline [24] (725 mg, 3.55 mmol), bis(pinacolato)diboron (1.1 g, 4.26 mmol) and potassium acetate (1.0 g, 10.66 mmol) in 1,4-dioxane (35 mL) was sparged with nitrogen for 5 min. Pd(dppf)Cl2¡¤DCM (174 mg, 0.21 mmol) was added and the mixture was heated under reflux for 4 h. The reaction was cooled to room temperature and concentrated under reduced pressure. The residue was diluted with EtOAc, filtered through Celite, then concentrated under reduced pressure to return the crude product which was purified by flash column chromatography, eluting with 0-50% EtOAc in isohexane, to return 49i (761 mg, 78%). 1H NMR (300 MHz, CDCl3) delta 6.90 (dd, J = 2.68, 9.18 Hz, 1H), 6.49 (dd, J = 2.64, 10.17 Hz, 1H), 2.33 (s, 3H), 1.36 (s, 12H).

According to the analysis of related databases, 502496-36-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Newton, Rebecca; Bowler, Katherine A.; Burns, Emily M.; Chapman, Philip J.; Fairweather, Emma E.; Fritzl, Samantha J.R.; Goldberg, Kristin M.; Hamilton, Niall M.; Holt, Sarah V.; Hopkins, Gemma V.; Jones, Stuart D.; Jordan, Allan M.; Lyons, Amanda J.; Nikki March; McDonald, Neil Q.; Maguire, Laura A.; Mould, Daniel P.; Purkiss, Andrew G.; Small, Helen F.; Stowell, Alexandra I.J.; Thomson, Graeme J.; Waddell, Ian D.; Waszkowycz, Bohdan; Watson, Amanda J.; Ogilvie, Donald J.; European Journal of Medicinal Chemistry; vol. 112; (2016); p. 20 – 32;,
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Adding a certain compound to certain chemical reactions, such as: 6274-57-3, name is 1-(4-Bromophenyl)-N,N-dimethylmethanamine, 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 6274-57-3, Safety of 1-(4-Bromophenyl)-N,N-dimethylmethanamine

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.

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-(4-Bromophenyl)-N,N-dimethylmethanamine, other downstream synthetic routes, hurry up and to see.

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;,
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