Category: bromides-buliding-blocks

Synthetic Route of 2270-59-9, 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. 2270-59-9, name is 5-Bromo-2-methylpent-2-ene, This compound has unique chemical properties. The synthetic route is as follows.

1.55 kg of magnesium and 10 kg of THF are charged into a stainless steel reactor provided with liquid nitrogen cooling . This is heated under reflux (60-700C) and, still at that temperature, 0.5 I of the solution containing 10 kg of 5-bromo-2-methyl- pentene (II) at 100% is poured. This is kept under reflux for at least 10 minutes until the reaction starts. The reaction mixture is then cooled to 50-600C and, keeping it at that temperature with a brine bath, the remaining solution of 5-bromo- 2-methyl-pentene (II) in THF is poured. The reaction mixture is kept at 50-600C for at least 1.5 hours and 40 kg of THF are added. The reaction mixture is then cooled with liquid nitrogen to -65/-700C and at that temperature 7.2 kg of diethyloxalate are added. The reaction mixture is kept at -65/-700C for at least 1 hour, under EPO stirring. The mixture thus obtained is then poured into another enamelled reactor containing 10kg of 32% hydrochloric acid dissolved in 30 kg of demineralised water and previously cooled to 0-100C.The reaction mixture is then brought to 20-300C and left until the phases separate. The aqueous phase is removed, while the organic phase is washed at 20-300C with 0.25 kg of sodium bicarbonate dissolved in 5 kg of demineralised water. The reaction mixture is stirred at the same temperature and left until the phases separate. The lower aqueous phase is removed, while the solvent is removed from the organic phase by vacuum distillation until an oily residue is obtained. Then 15 kg of THF are added and the mixture obtained is stirred until a solution is obtained which is sent to the next stage. Yield not determined.

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

Reference:
Patent; ERREGIERRE S.p.A.; STRAGEN PHARMA SA; WO2007/9953; (2007); A1;,
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Reference of 73918-56-6,Some common heterocyclic compound, 73918-56-6, name is 2-(4-Bromophenyl)ethanamine, molecular formula is C8H10BrN, 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. BOC2O (818 mg, 3.75 mmol, 1.5 eq.) was added to a stirred solution of 2-(4- bromophenyl)ethanamine (500 mg, 2.5 mmol, 1.0 eq.) and TEA (1.5 ml, 7.5 mmol, 3.0 eq.) in DCM (25 ml) at 0 0C and resulting reaction mixture is stirred at 25 0C for 6 h. The reaction mixture was diluted with DCM (75 ml), washed with water (2 x 50 ml) and brine (50 ml) and dried over Na2SO4. The solvent was evaporated under reduced pressure and the residue triturated with hexanes to yield the desired product as an off white solid.Yield: 100 % (750 mg, 2.5 mmol)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(4-Bromophenyl)ethanamine, its application will become more common.

Reference:
Patent; GRUeNENTHAL GMBH; MERLA, Beatrix; OBERBOeRSCH, Stefan; REICH, Melanie; SCHUNK, Stefan; JOSTOCK, Ruth; HEES, Sabine; ENGELS, Michael; GERMANN, Tieno; BIJSTERVELD, Edward; WO2010/99938; (2010); A1;,
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Reference of 2550-36-9, 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. 2550-36-9, name is (Bromomethyl)cyclohexane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

20 g of bromomethyl cyclohexane,After 12.5 g of 1-naphthol was dissolved in 300 g of NMP in a three-necked flask,12g of potassium carbonate was added,14g potassium iodide was heated at 120 C for 8 hours.In the reaction solution was added 300g of water,Extraction was performed three times with 100 g of hexane,The resulting organic layers were combined,Washed once with 100 g of 1 N aqueous sodium hydroxide solution,Water 100g washed once,Brine 100g washed once,Concentration gave 13 g of compound 1.

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

Reference:
Patent; FUJIFILM CORPORATION; SHIRAKAWA, MICHIHIRO; TANGO, NAOHIRO; SHIBUYA, AKINORI; YAMAGUCHI, SHUHEI; KATAOKA, SHOHEI; (175 pag.)TWI579263; (2017); B;,
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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. 21524-34-5, name is 2-Bromo-1,3,5-triisopropylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Bromo-1,3,5-triisopropylbenzene

General procedure: Ligand comparison reactions were setup at the same time using the same batches of reagents. In a N2 filled glove-box, a microwave vialwas charged with a magnetic stir bar, Pd2(dba)3 (2.3 mg, 0.0025mmol), the respective ligand L1-L5 (0.010 mmol), K3PO4 (424 mg, 2.00 mmol), and 2-biphenyboronic acid (9; 158 mg, 0.800 mmol). Degassed (argon sparge) toluene (1.3 mL) followed by bromide 8 (0.169 mL, 0.667 mmol) were added, and the vial was sealed with acrimp-cap septum and removed from the glove-box. The reaction vialwas then inserted into a heating block pre-heated to 80 C. Aliquots were removed using argon-purged syringes and quenched into MeOH and analyzed by UPLC. After complete consumption of the starting aryl bromide (2 h), the reaction mixture was cooled to r.t. and partitioned between H2O and CH2Cl2. The organic layer was collected,dried (anhyd Na2SO4), and concentrated in vacuo. The yield of thecrude mixture was determined by 1HNMR spectroscopy using dimethyl fumarate as the analytical standard.

According to the analysis of related databases, 21524-34-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Yongda; Lao, Kendricks S.; Sieber, Joshua D.; Xu, Yibo; Wu, Linglin; Wang, Xiao-Jun; Desrosiers, Jean-Nicolas; Lee, Heewon; Haddad, Nizar; Han, Zhengxu S.; Yee, Nathan K.; Song, Jinhua J.; Howell, Amy R.; Senanayake, Chris H.; Synthesis; vol. 50; 22; (2018); p. 4429 – 4434;,
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Synthetic Route of 4263-52-9, A common heterocyclic compound, 4263-52-9, name is Sodium 2-bromoethanesulphonate, molecular formula is C2H4BrNaO3S, 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.

General procedure: A solution of 1mmol of chloride salt 1a or 2a in distilled water was treated with equimolar quantity of various salts (NaBF4, KPF6, 2-BrCH2CH2SO3Na). The reaction mixture was stirred at room temperature for 12h. Next, the reaction mixture was extracted twice with CH2Cl2. The organic layer was dried over anhydrous Na2SO4 and then CH2Cl2 was evaporated on a rotary evaporator to give various chiral ionic liquids 1b-d and 2b-d. 4.4.6 1-[(-)-Borneoxycarbonylmethylene]-3-methyl benzimidazolium 2-bromoethylsulfonate [ABoMBI]OSO2CH2CH2Br 2d Off-white solid Yield = 83%, mp = 96-98 C, [alpha]D25 = -15.6 (c 0.25, EtOH). 1H NMR (CDCl3, 400 MHz): delta 10. 35 (s, 1H), 7.78-7.68 (d, 1H, Ar), 7.60 (s, 3H, Ar), 5.47 (s, 2H NCH2), 5.44-5.35 (d, 1 H), 4.13 (s, 3H N-CH3), 3.60-3.52 (t, 2H), 3.20-3.07 (t, 2H), 2.31-2.19 (m, 1H), 1.72-1.56 (m, 3H), 1.19 (s, 3H), 1.02-0.97 (d, 1H), 0.80 (s, 6H), 0.74 (s, 3H). 13C NMR (CDCl3, 400 MHz): delta 166.09, 144.39, 131.67, 131.47, 127.46, 127.32, 113.07, 112.93, 83.16, 54.40, 48.93, 47.91, 44.64, 36.34, 33.76, 29.59, 27.79, 26.87, 26.29, 19.58, 18.72, 13.47. EI-MS: m/z = 327 [M+cation], m/z = 312 [M+cation-CH3].

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; Singh, Avtar; Chopra, Harish Kumar; Tetrahedron Asymmetry; vol. 27; 11-12; (2016); p. 448 – 453;,
Bromide – Wikipedia,
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Synthetic Route of 766-46-1, These common heterocyclic compound, 766-46-1, name is 2′-Bromophenylacetylene, 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.

General procedure: An oven dried 20 mL glass vial was charged with PdCl2(PPh3)2 (28.1 mg, 0.04 mmol), CuI (7.6 mg, 0.04 mmol), acid chloride (2.60 mmol), terminal alkyne (2.00 mmol) and anhydrous triethylamine (10 mL). The vial was flushed with nitrogen and sealed with a pressure relief cap. The reaction mixture was stirred at room temperature, overnight, until the disappearance of starting material was observed, as monitored by thin layer chromatography. The reaction mixture was diluted with diethyl ether (40 mL) and washed with brine (40 mL). The aqueous phase was then extracted with diethyl ether (2 x 20 mL). The combined organic layers were dried over anhydrous MgSO4, and concentrated using a rotary evaporator under reduced pressure (20 mmHg). The resulting residue was purified by flash column chromatography on silica gel (eluent: hexanes/ethyl acetate).

The synthetic route of 766-46-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liu, Xiaochen; Hong, Dongsub; She, Zhigang; Hersh, William H.; Yoo, Barney; Chen, Yu; Tetrahedron; vol. 74; 45; (2018); p. 6593 – 6606;,
Bromide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 51376-06-8, name is 5-Bromobenzo[c][1,2,5]oxadiazole, 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 51376-06-8, Computed Properties of C6H3BrN2O

5-bromo-2,1,3-benzoxadiazole (0.71 g), cesium carbonate (1.4 g), 2,2′- bis(diphenylphosphino)-1,r-binapthyl (0.17 g) and Tris-(dibenzylideneacetone) dipalladium(O) (0.13g) were added to a solution of (5S)-3-[3-fluoro-4-(piperidin-4- yloxy)phenyl]-5-[(isoxazol-3-ylamino)methyl]-1,3-oxazolidin-2-one (1.3 g) (obtained from Step b) in dry dimethylformamide (15 mL) and the reaction mixture was heated at 100 C for about 17 hours. The reaction mixture was filtered and the solvent was evaporated. The crude product thus obtained was purified by column chromatography using 1 % methanol in dichloromethane to yield the title product (0.07g).Melting point: 75-100 C; EIMS (m/z): 534.21; 1HNMR(DMSO): delta 8.16 (s, 1H), 7.66 (d, 1H), 7.48 (dd, 1H), 7.3 (m, 2H), 7.17 (d, 1H), 7.08-7.05 (t, 1H), 6.75 (s, 1H), 4.99 (m, 1H), 4.53 (m, 3H), 4.14-4.11 (t, 1H), 3.95 (t, 1H), 3.61 (m, 2H), 3.3 (m, 2H), 2.04 (m, 4H).

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-Bromobenzo[c][1,2,5]oxadiazole, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; RANBAXY LABORATORIES LIMITED; WO2006/35283; (2006); 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. 5433-01-2, name is 1-Bromo-3-isopropylbenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 5433-01-2

Preparation Example 1-1: Preparation of 4-t-butyl-N- (4- isopropylphenyl ) benzenamine; As represented below in Reaction Scheme 1, 25g of 3-t- butylaniline (0.125mol) and 37.3g of 3-bromoisopropylbenzene(0.25mol) were dissolved in 25OmL of toluene, and 3.43g ofPd2(dba)3 (0.0037mol) was added thereto under a nitrogen atmosphere. Then, 14.4g of NaOBufc (0.15mol) and 1.157g of (t- Bu)3P (0.0075mol) were added to the reaction solvent, and the reaction mixture was refluxed and stirred for 12 hours. The reaction mixture was checked for the completion of the reaction by means of TLC, and if the reaction was completed, the reaction product was cooled down to room temperature. The reacted solution was poured onto a thin silica pad to perform short chromatography, and then was washed with methylene chloride (MC) . The washed solution was subjected to distillation under reduced pressure to thereby remove the solvent, and was chromatographed using n-hexane to thereby obtain a desired white solid product (29.4g, 88%). [Reaction Scheme 1]

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; DOOSAN CORPORATION; WO2009/91095; (2009); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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 4101-68-2 as follows. name: 1,10-Dibromodecan

2.2.4 9-(10-bromodecyl)-9H-carbazole (4) Under argon atmosphere, carbazole (1.67 g, 0.01 mol), anhydrous potassium carbonate (2.77 g, 0.02 mol), and 1,10-dibromodecane (6.00 g, 0.02 mol) in 40 mL of anhydrous acetonitrile were refluxed at 95 C for 36 h. After cooling to room temperature, insoluble substance was filtered, and the solvent was removed under reduced pressure. The crude product was purified by column chromatography on silica gel with petroleum to get 9-(10-bromodecyl)-9H-carbazole as white crystals (1.66 g, Yield 43%). 1H NMR (500 MHz, CDCl3, delta): 8.08 (d, J = 7.7 Hz, 2H, Ar-H), 7.43 (t, J = 7.8 Hz, 2H, Ar-H), 7.35 (d, J = 8.1 Hz, 2H, Ar-H), 7.20 (t, J = 7.5 Hz, 2H, Ar-H), 4.21 (t, J = 7.3 Hz, 2H, CH2), 3.33 (t, J = 6.8 Hz, 2H, CH2Br), 1.79 (m, 4H, CH2), 1.33-0.91 (m, 12H, CH2). FT-IR (cm-1, KBr): 2930, 2850 (s; CH), 1632, 1619, 1593 (m; Ar). Anal. Calcd. For C22H28BrN: C, 68.39; H, 7.30; N, 3.63; Found: C, 68.47; H, 7.25; N, 3.56.

According to the analysis of related databases, 4101-68-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Huang, Jin; Wang, Weina; Gu, Jiangjiang; Li, Weizhi; Zhang, Qiuhong; Ding, Yin; Xi, Kai; Zheng, Youxuan; Jia, Xudong; Polymer; vol. 55; 26; (2014); p. 6696 – 6707;,
Bromide – Wikipedia,
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Application of 10485-09-3, These common heterocyclic compound, 10485-09-3, name is 2-Bromoindene, 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.

(Comparative Example 3) 1.2 ml of a tetrahydrofuran solution of 0.25 g of magnesium was cooled to 0C, and 5.0 ml of a tetrahydrofuran solution of 1.0 g of 2-bromoindene was slowly dropped thereto.After the dropping, the mixture was stirred at the same temperature for 1 hour, and 0.57 g of 2,6- dimethylbenzaldehyde was added thereto, and stirred for 12 hours while the temperature was being raised to 25C.After the confirmation of the degree of reaction progress by TLC, the reaction was terminated with an ammonium chloride aqueous solution, and an organic phase was extracted with ethyl acetate.[0132] After the obtained organic phase was dried with anhydrous magnesium sulfate, the organic phase was concentrated and purified by column chromatography. Then, 5 g of manganese dioxide was added to 30 ml of a chloroform solution of the obtained intermediate compound, and the mixture was stirred at 25 C for 12 hours. After the confirmation of the degree of reaction progress by TLC, the manganese dioxide was filtered, and 0.42 g (yield: 40%) of Comparative Product 3 shown below was obtained by recrystallization. Thestructure of Comparative Product 3 was confirmed by 1HNMR. 1H-NMR (CDC13; TMS) : delta 2.21 (s, 6H) , 3.85 (s, 2H) , 7.07 (d, 2H) , 7.20-7.26 (m, 2H) , 7.33-7.41 (m, 2H) , 7.47 (d, 1H) , 7.58 (d, 1H)

The synthetic route of 10485-09-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CANON KABUSHIKI KAISHA; SAITOH, Terunobu; WO2011/81078; (2011); A1;,
Bromide – Wikipedia,
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