Bromides-buliding-blocks

344-03-6, 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 344-03-6 as follows.

Unitine , 4 -bromotetrafluorobenzene, 0.11 muM 1 unitunitunito-cyanophenylboronic acid 0.1 muM 4 – 0 . 001molPd under a nitrogen atmosphere2(Dba)3Unitunitunits, 0.002 muM s-phos, 0 . 2molK3PO4The unitz reacted 300 ml 12h. 100 ml was found in a mixed solution consisting of unit_transformants ‘-type 100 C’-type ‘.’. Obtained M1

According to the analysis of related databases, 1,4-Dibromotetrafluorobenzene, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Beijing Dingcai Technology Co., Ltd.; Tsinghua University; Duan Lian; Zhang Dongdong; Song Xiaozeng; Gao Wenzheng; Huang Xinxin; (33 pag.)CN110066227; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary

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. 1647-26-3 name is 1-Bromo-2-cyclohexylethane, 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. 1647-26-3

Combine 6- (4-Piperidin-3-yl-phenoxy)-nicotinamide (free base compound of example 322) (0.0255g, 0.0858 MMOL), 1-BROMO-2-CYCLOHEXYLETHANE (0.0150 mL, 0.0958 mmol), and potassium carbonate (0.0245 g, 0.177 mmol) in dimethylformamide (1.0 mL) and stir for 10 min. Purify the reaction mixture by ion exchange chromatography (SCX resin, METHANOL- 2 M AMMONIA/METHANOL) and silica gel chromatography (15: 1 No. 10: 1 ethyl acetate: methanol) to provide 0.0146 g (42%) of the title compound as an off-white foam: high resolution mass spectrum (electrospray): m/z calc for C25H34N302 408. 2651, found 408.2661 ; H NMR (methanol-d4): 8.61 (s br, 1H), 8. 28 (d, 1H, J= 7.8 Hz), 7.36 (d, 2H, J= 7.8 Hz), 7.12 (d, 2H, J= 7.8 Hz), 7.01 (d, 1H, J = 8.3 Hz), 3.07 (d, 2H, J = 10.2 Hz), 2.89 (t, 1H, J= 11.2 Hz), 2.55-2. 42 (M, 2H), 2.15-1. 93 (m, 4H), 1.93-1. 64 (m, 8H), 1.63-1. 43 (m, 4H), 1.40-1. 15 (m, 8H), 1.07-0. 86 (m, 3H).

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

Reference:
Patent; ELI LILLY AND COMPANY; WO2004/26305; (2004); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

22385-77-9, Adding some certain compound to certain chemical reactions, such as: 22385-77-9, name is 1-Bromo-3,5-di-tert-butylbenzene, 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 22385-77-9.

General procedure: To a solution of phthalimide (20 mmol) in CH2Cl2 (70 mL) was added the Grignard reagent (preformed from 50 mmol ArBr, 60 mmol mg in 30 mL THF) at room temperature. The resulting mixture was stirred at room temperature for 1.5 h and quenched with saturated aqueous solution of NH4Cl (40 mL). Then the mixture was extracted with ethyl acetate and washed with brine. The collected organic phase was dried over anhydrous Na2SO4 and concentrated under vacuum. The residue was purified by chromatography, eluting with ethyl acetate/petroleum ether 1:1 (v/v), to afford the 3-aryl-3-hydroxyisoindolin-1-ones.

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 22385-77-9.

Reference:
Article; Ge, Chen; Liang, Ren-Xiao; Liu, Ren-Rong; Xiang, Bin; Jia, Yi-Xia; Tetrahedron Letters; vol. 58; 2; (2017); p. 142 – 144;,
Bromide – Wikipedia,
bromide – Wiktionary

55289-36-6, The chemical industry reduces the impact on the environment during synthesis 55289-36-6, name is 3-Bromo-2-methylaniline, I believe this compound will play a more active role in future production and life.

31 mL of 1N sulfuric acid aqueous solution was added to 3-bromo-2-methylaniline (4.04 g, 21.7 mmol), andthe mixture was cooled to 0C. Sodium nitrite (6.0 M aqueous solution, 4.3 mL) was slowly added thereto. After 15minutes, 10 mL of sulfuric acid was added thereto, and the mixture was stirred for 1 hour under reflux. The reactionsolution was cooled to room temperature. After addition of water, the reaction solution was extracted with Et2O. Theorganic layer was dried with anhydrous magnesium sulfate and purified by column chromatography to obtain the titlecompound (2.34 g, 58 %).1H-NMR (CDCl3) delta 7.14 (1H, d), 6.92 (1H, t), 6.71 (1H, d), 4.83 (1H, brs), 2.34 (3H, s)

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

Reference:
Patent; LG Chem, Ltd.; KIM, Young Kwan; PARK, Sang Yun; JOO, Hyun Woo; CHOI, Eun Sil; PAEK, Seung Yup; KANG, Seung Wan; KIM, Byung Gyu; LEE, Chang Seok; KIM, Sung Wook; LEE, Sang Dae; (369 pag.)EP3239143; (2017); A2;,
Bromide – Wikipedia,
bromide – Wiktionary

Some common heterocyclic compound, 2695-47-8, name is 6-Bromo-1-hexene, molecular formula is C6H11Br, 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. 2695-47-8

Step A: Preparation of 2,2,2-trifluoro-N-(hex-5-enyl)-N-methylacetamide 1a. At 0 C. and under nitrogen atmosphere, sodium hydride (60% dispersion in mineral oil, 31.5 g, 1.28 eq.) was slowly added to a cooled solution of N-methyl-2,2,2-trifluoroacetamide (100 g, 1.28 eq.) in DMF (500 mL). The reaction mixture was stirred for 2 hrs at 0 C. and 6-bromo-1-hexene (100 g, 1 eq.) was added dropwise for 45 min. The reaction mixture was allowed to warm up to room temperature and was stirred for 3 days. The reaction mixture was poured into water and extracted three times with EtOAc. The combined organic layers were dried over anhydrous sodium sulphate, and evaporated under reduced pressure. The resulting residue was purified by chromatography on silica gel (petroleum ether/EtOAc) to yield compound 1a as colourless oil in 56% yield. 1H NMR (DMSO-d6, 400 MHz) delta (ppm) 1.27-1.38 (m, 2H), 1.48-1.60 (m, 2H), 2-2.06 (m, 2H), 2.93 (m, 3H), 3.35-3.40 (m, 2H), 4.92-5.04 (m, 2H), 5.73-5.83 (m, 1H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2695-47-8, its application will become more common.

Reference:
Patent; Idenix Pharmaceuticals, Inc.; US2010/260710; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

These common heterocyclic compound, 3814-30-0, name is (Bromomethyl)cyclopentane, 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. 3814-30-0

EXAMPLE 136 4-(4-Chloro-3-cyclopentylmethylsulfamoylphenyl)-3-methyl-2-methylimino-1,3-thiazolidine-4-ole 6.7 g of 4-(4-Chloro-3-sulfamoylphenyl)-3-methyl-2-methylimino-1,3-thiazolidine-4-ole (Example 2) were introduced, while stirring, into a mixture of 10 ml of absolute dimethyl sulfoxide and 1.2 g of pulverized potassium hydroxide with the exclusion of nitrogen, the temperature being maintained between 8 C and 12 C by outward cooling. While cooling and stirring were maintained, 3.3 g of cyclopentylmethylbromide were added dropwise, the mixture was stirred for 10 hours at room temperature and precipitated with 100 ml of water. The oily residue was decanted, the amorphous product was solidified under 100 ml of fresh water, suction-filtered and washed with water several times. Yellow-brown solid substance, decomposition beginning at 72 C. The IR-spectrum was identical with that of Example 76.

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 3814-30-0.

Reference:
Patent; Hoechst Aktiengesellschaft; US4061761; (1977); A;,
Bromide – Wikipedia,
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. 4549-32-0, name is 1,8-Dibromooctane belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. 4549-32-0

General procedure: To a stirred solution of n-dibromoalkane (1 equiv.) in anhydrous THF (0.1M) under an argon atmosphere was added tert-BuOK (1.15 equiv.) in portionwise over 30 min. After being stirred under reflux for 16h, the reaction was cooled and subsequently quenched with water. The resulting mixture was then diluted with diethylether, and the layers were separated. The aqueous layer was extracted several times with diethylether, and the combined organic layers were washed with brine, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The resultant crude product was purified by flash column chromatography over silica gel using petroleum ether as eluent to afford the desired product.

The synthetic route of 4549-32-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Saied, Essa M.; Le, Thuy Linh-Stella; Hornemann; Arenz, Christoph; Bioorganic and Medicinal Chemistry; vol. 26; 14; (2018); p. 4047 – 4057;,
Bromide – Wikipedia,
bromide – Wiktionary

39478-78-9, Adding some certain compound to certain chemical reactions, such as: 39478-78-9, name is 5-Bromo-2-methylaniline, 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 39478-78-9.

General procedure: In a typical run, h-BN(at)Fur(at)Pd(OAc)2 (0.05 mmol) was added to a mixture of arylboronic acid 1 (1.0 mmol), aryl bromide 2 (1.5 mmol) and K2CO3 (1.5 mmol) in water (1 mL). The resulting mixture was stirred at 70 C under Ar protection, and the progress of the reaction was monitored by TLC. After completion of the reaction, ethyl acetate was added to the reaction mixture and the catalyst was separated. The organic phase was washed with water, dried over anhydrous Na2SO4 and the solvent was evaporated under reduced pressure. Finally, the residue was isolated by chromatography on a column of silica gel to afford the corresponding product 3.

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 39478-78-9.

Reference:
Article; Li, Weijian; Lv, Guanghui; Cheng, Xu; Sang, Rui; Ma, Xiaojun; Zhang, Yong; Nie, Ruifang; Li, Jie; Guan, Mei; Wu, Yong; Tetrahedron; vol. 72; 52; (2016); p. 8557 – 8564;,
Bromide – Wikipedia,
bromide – Wiktionary

A common heterocyclic compound, 1646-54-4, name is 1,4-Dibromo-2,3,5,6-tetramethylbenzene, molecular formula is C10H12Br2, 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. 1646-54-4.

The reaction pathway is shown in Scheme 1. H4dbtec ligand was prepared according literature [13] and with a little modification. To a four-necked flask equipped with a reflux condenser and a mechanical stirrer, 3,6-bromo-tetramethylbenzene (0.171 mol), 2.1 L pyridine and 280 mL water were added. The reaction mixture was heated to 100 C while stirring. KMnO4 (0.859 mol) was added in small portions and the mixture was refluxed for 5 h. The warm solution was separated from MnO2 by filtration and the solvent evaporated under reduced pressure. 280 mL water and 112 g NaOH were added to the residual solid. After the combined mixture was heated up to 100 C, KMnO4 (0.859 mol) was added again in small portions and the mixture was refluxed for 5 h. The excess KMnO4 was destroyed by the cautious addition of 140 mL ethanol. The MnO2 was removed from the hot mixture by filtration. The filtrate was acidified with aqueous HCl (5 M, 600 mL). After the solvent was revaporated, the residue was washed with acetone. The resultant solid was dried. The yield was 46 g (66%). 1H NMR (300 MHz; DMSO-d6) no signals. 13C NMR (100 MHz; DMSO-d6) deltac 115.51, 137.57, 166.27.

The synthetic route of 1,4-Dibromo-2,3,5,6-tetramethylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Liang-Liang; Guo, Yu; Wei, Yan-Hui; Guo, Jie; Wang, Xing-Po; Sun, Dao-Feng; Journal of Molecular Structure; vol. 1038; (2013); p. 73 – 77;,
Bromide – Wikipedia,
bromide – Wiktionary

The chemical industry reduces the impact on the environment during synthesis 28342-75-8, name is 1,5-Dibromo-2,4-difluorobenzene, I believe this compound will play a more active role in future production and life. 28342-75-8

l,5-Dibromo-2,4-difluorobenzene (1, 1.36 g, 5.00 mmol) was dissolved in dry diethyl ether ( 15 mL) and cooled down to -78C. 2.35 M n-Butyllithium in hexane (2.20 mL, 5.25 mmol) was added drop-wise with stirring . After 15 minutes, dry N,N- dimethylformamide (0.77 mL, 10.0 mmol) was added and the resulting mixture was stirred at for 15 minutes and then allowed to warm to ambient temperature. After one hour, the reaction mixture was quenched with 1.0 M aqueous solution of hydrochloric acid ( 15 mL) . Layers were separated and the organic layer was washed with brine ( 15 mL), dried over anhydrous magnesium sulfate and evaporated . The residue was purified by flash column chromatography (Silicagel 60, 0.063-0.200 mm ; eluent: cyclohexane/ ethyl acetate 20 : 1) 5-bromo-2,4-difluorobenzaldehyde (2) as colorless oil which solidified on storage in freezer. Yield : 780 mg (70%) . JH NM R spectrum (300 MHz, CDCI3, deltaEta) : 10.26 (s, 1 H) ; 8.14 (dd, J =9.6 and 8.0 Hz, 1 H) ; 7.05 (d, J = 8.0 Hz, 1 H) .

The chemical industry reduces the impact on the environment during synthesis 28342-75-8. I believe this compound will play a more active role in future production and life.

Reference:
Patent; NOVO NORDISK A/S; KRUSE, Thomas; HANSEN, Mikael, Kofoed; MUeNZEL, Martin, Werner, Borchsenius; TH?GERSEN, Henning; SAUERBERG, Per; RASMUSSEN, Jakob, Ewald; BEHRENS, Carsten; H?EG-JENSEN, Thomas; BAL?ANEK, Vojtech; DROBNAKOVA, Zuzana; DRO?, Ladislav; HAVRANEK, Miroslav; KOTEK, Vladislav; ?TENGL, Milan; ?NAJDR, Ivan; VANOVA, Hana; (202 pag.)WO2019/92125; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary