Sep-21 News New downstream synthetic route of 40422-70-6

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.

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. 40422-70-6, name is 1-Bromo-3-(2-bromoethyl)benzene, A new synthetic method of this compound is introduced below., name: 1-Bromo-3-(2-bromoethyl)benzene

To a solution of 3-bromophenethylbromide (1 g, 3.83 mmol) in DMF (10 mL) was added 40% aqueous methylamine (2.97 mL, 38.3 mmol), followed by Cs2CO3 (1.625 g, 5 mmol). After the reaction mixture was refluxed for 1 h, it was cooled to room temperature and the solvent was removed. The residue was dissolved in ethyl acetate (30 mL), and the organic layer was washed with water (3 × 20 mL) and dried over Na2SO4. The solvent was removed in vacuo, and the oily residue was further purified using flash column chromatography (CHCl3/MeOH 5:2) yielding in 2 (100 mg, 12%) as a colorless liquid. 1H NMR (300 MHz, CDCl3): delta 7.26-7.23 (m, 2H, ArH), 7.06-7.04 (m, 2H, ArH), 2.78-2.74 (m, 4H), 2.30 (s, 3H, NCH3); TLC Rf: 0.2 (CHCl3/MeOH 5:2); GC-MS (EI) m/z (% rel Int.): 214 (100.0 [M]+), rt: 7.240 min (full analytical data are reported in27).

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; Herth, Matthias M.; Hansen, Hanne D.; Ettrup, Anders; Dyssegaard, Agnete; Lehel, Szabolcs; Kristensen, Jesper; Knudsen, Gitte M.; Bioorganic and Medicinal Chemistry; vol. 20; 14; (2012); p. 4574 – 4581;,
Bromide – Wikipedia,
bromide – Wiktionary

22-Sep-2021 News Discovery of 40422-70-6

The synthetic route of 40422-70-6 has been constantly updated, and we look forward to future research findings.

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. 40422-70-6, name is 1-Bromo-3-(2-bromoethyl)benzene, A new synthetic method of this compound is introduced below., Computed Properties of C8H8Br2

A mixture of 2,4,6-trimethyl-N-((3′-(methylsulfonyl)-[l, r-biphenyl]-4- yl)methyl)benzenesulfonamide (0.443 g, 1 mmol), K2CO3 (0.276 g, 2 mmol), and l-bromo-3-(2-bromoethyl)benzene (0.792 g, 3 mmol) in anhydrous acetonitrile (5 ml) was heated to 85 C for 2 h under microwave irradiation. The white powder was filtered off, the solvent was evaporated and the mixture was dissolved in ethyl acetate and extracted with brine. The organic phase was separated, dried over anhydrous MgS04, filtered and concentrated in vacuo. The remaining crude residue was purified by flash chromatography on silica gel (ethyl acetate/hexanes) to obtain the title compound as white sharp needles (88% based on recovery of the starting materials); FontWeight=”Bold” FontSize=”10″ H NMR (400 MHz, Chloroform-Patent; THE SCRIPPS RESEARCH INSTITUTE; KAMENECKA, Theodore, Mark; BURRIS, Thomas; WO2014/85453; (2014); A2;,
Bromide – Wikipedia,
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Continuously updated synthesis method about 40422-70-6

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

Reference of 40422-70-6, 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. 40422-70-6, name is 1-Bromo-3-(2-bromoethyl)benzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 18; 4-Bromo-2-(2-bromo-ethyl)-benzenesulfonyl chlorideChlorosulfonic acid (17 mL) was added dropwise to 1-bromo-3-(2-bromo-ethyl)-benzene (5 g, 19 mmol) at 0 C. The mixture was stirred at 0 C. for 1 h then an additional 3 h at rt. The mixture was poured into an ice-water slowly and extracted with methylene chloride, and the combined organic layers were evaporated under reduced pressure to give 4.3 g of crude 4-Bromo-2-(2-bromo-ethyl)-benzenesulfonyl chloride which was used directly for next reaction. MS (ESI) 342.9 (M-Cl+OH)-.

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

Reference:
Patent; Roche Palo Alto LLC; US2010/16302; (2010); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Introduction of a new synthetic route about 1-Bromo-3-(2-bromoethyl)benzene

Statistics shows that 1-Bromo-3-(2-bromoethyl)benzene is playing an increasingly important role. we look forward to future research findings about 40422-70-6.

Synthetic Route of 40422-70-6, These common heterocyclic compound, 40422-70-6, name is 1-Bromo-3-(2-bromoethyl)benzene, 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: Table 3 is a parameter table. The starting material “parameter 1” was added into a flask at room temperature under N2, and then the “parameter 2” mL IPA and “parameter 3” were added thereinto. The starting material was dissolved at “parameter 4” C. The appearances of reaction solution were “parameter 5” and “parameter 7” in about “parameter 6” minutes, and then the solution was heated at 110~120C for “parameter 8” hours and concentrated in room temperature. The “parameter 9” mL MeOH was added and the resulting mixture was stirred for “parameter 10” minutes. To the solution, which is “parameter 1 1” in a ice-bath, NaBH4(s) “parameter 12” was added slowly under N 2 and stirred for “parameter 13” minutes. The solution, which is “parameter 14,” was added with “parameter 15” mL H2O and extracted with “parameter 16” mL CHC13. The organic layer was added with MgS04 for drying, stirred for “parameter 17” minutes, filtered, and concentrated to obtain “parameter 18”. The “parameter 20” was afforded after flash column chromatography (silica gel, “parameter 19”).

Statistics shows that 1-Bromo-3-(2-bromoethyl)benzene is playing an increasingly important role. we look forward to future research findings about 40422-70-6.

Reference:
Patent; YU, Linda Chia-Hui; HSIN, Ling-Wei; LEE, Tsung-Chun; (0 pag.)WO2018/157233; (2018); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

New downstream synthetic route of 40422-70-6

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.

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. 40422-70-6, name is 1-Bromo-3-(2-bromoethyl)benzene, A new synthetic method of this compound is introduced below., category: bromides-buliding-blocks

To a solution of 3-bromophenethylbromide (1 g, 3.83 mmol) in DMF (10 mL) was added 40% aqueous methylamine (2.97 mL, 38.3 mmol), followed by Cs2CO3 (1.625 g, 5 mmol). After the reaction mixture was refluxed for 1 h, it was cooled to room temperature and the solvent was removed. The residue was dissolved in ethyl acetate (30 mL), and the organic layer was washed with water (3 × 20 mL) and dried over Na2SO4. The solvent was removed in vacuo, and the oily residue was further purified using flash column chromatography (CHCl3/MeOH 5:2) yielding in 2 (100 mg, 12%) as a colorless liquid. 1H NMR (300 MHz, CDCl3): delta 7.26-7.23 (m, 2H, ArH), 7.06-7.04 (m, 2H, ArH), 2.78-2.74 (m, 4H), 2.30 (s, 3H, NCH3); TLC Rf: 0.2 (CHCl3/MeOH 5:2); GC-MS (EI) m/z (% rel Int.): 214 (100.0 [M]+), rt: 7.240 min (full analytical data are reported in27).

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; Herth, Matthias M.; Hansen, Hanne D.; Ettrup, Anders; Dyssegaard, Agnete; Lehel, Szabolcs; Kristensen, Jesper; Knudsen, Gitte M.; Bioorganic and Medicinal Chemistry; vol. 20; 14; (2012); p. 4574 – 4581;,
Bromide – Wikipedia,
bromide – Wiktionary

Some tips on 40422-70-6

According to the analysis of related databases, 40422-70-6, the application of this compound in the production field has become more and more popular.

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. 40422-70-6, name is 1-Bromo-3-(2-bromoethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1-Bromo-3-(2-bromoethyl)benzene

To a 100 ml three neck round bottomed flask under nitrogen atmosphere, (R)-2- isopropyl-3,6-dimethoxy-2,5-dihydropyrazine (4 g, 21.7 mmol) was dissolved in dry THF (28 ml) and cooled to -78 C. To this reaction mixture, 1 .6 M solution of n-BuLi in hexanes (16.3 ml, 26 mmol) was added dropwise at -78 C and stirred for 15 minutes. A solution of l-bromo-3- (2-bromoethyl)benzene (5.73 g, 21 .7 mmol) in dry THF (13 ml) was added dropwise at -78 C and stirred for 1 h followed by stirring at rt for 3 h. The reaction mixture was quenched with saturated ammonium chloride solution and extracted using ethyl acetate. The combined organic layer was dried over sodium sulfate and concentrated and purified by flash column purification with 1 -3 % ethyl acetate in hexanes to yield 3.3 g of (2S,5R)-2-(3-bromophenethyl)-5-isopropyl- 3,6-dimethoxy-2,5-dihydropyrazine.

According to the analysis of related databases, 40422-70-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BRAMELD Kenneth; OWENS Timothy; WO2015/195950; A1; (2015);,
Bromide – Wikipedia,
bromide – Wiktionary

A new synthetic route of 40422-70-6

Statistics shows that 1-Bromo-3-(2-bromoethyl)benzene is playing an increasingly important role. we look forward to future research findings about 40422-70-6.

Application of 40422-70-6, These common heterocyclic compound, 40422-70-6, name is 1-Bromo-3-(2-bromoethyl)benzene, 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.

To prepare Fen-Br Meta, N-phenyl-N-piperidin-4-yl-propionannide (Norfentanyl, 0.93 g, 4.0 mmol) and 3-bromophenethyl bromide (1.58 g, 6.0 mmol) were dissolved in 15 mL DMF, followed by addition of N,iV-diisopropylethylamine (0.78 g, 6.0 mmol). The reaction was kept stirring at 60 C for 24 hours. The reaction mixture was cooled to room temperature before ethyl ether (100 mL) was added, and the organics were washed with 1 N NaOH (30 mL x 3), water (30 mL x 3) and brine (30 mL x 3). The organics were then dried over MgS04 and concentrated under vacuum. The organics were redissolved in ethyl ether, and pure Fen-Br was precipitated as HCl salt by addition of HCl in ethanol solution. Fen-Br Meta (93%). NMR (500 MHz, CDCb): delta 7.55-7.35 (m, 5H), 7.18 (dd, J = 8.5, 8.5 Hz, 2H), 7.09 (d, J = 8.5 Hz, 2H), 4.80 (tt, J = 12.0, 4.0 Hz, 1H), 3.62 (d, / = 12.0 Hz, 2H), 3.12 (m, 2H), 2.89 (td, J = 12.0, 1.5 Hz, 2H), 2.2-1.8 (m, 6H), 1.42 (m, 2 H), 1.01 (t, / = 7.5 Hz, 3H).

Statistics shows that 1-Bromo-3-(2-bromoethyl)benzene is playing an increasingly important role. we look forward to future research findings about 40422-70-6.

Reference:
Patent; ALLEGHENY-SINGER RESEARCH INSTITUTE; AVERICK, Saadyah; BADR, Ahmed; LI, Shaohua; LEJEUNE, Keith; (83 pag.)WO2017/41095; (2017); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

A new synthetic route of 1-Bromo-3-(2-bromoethyl)benzene

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.

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. 40422-70-6, name is 1-Bromo-3-(2-bromoethyl)benzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-3-(2-bromoethyl)benzene

General procedure: Thiourea (7 mmol) was dissolved in 13.5 mL ethanol and the appropriate alkylbromide (7 mmol) was added. The mixture was stirred and heated under reflux for 2 h after which the reaction became homogenous. The reaction was allowed to cool to room temperature and the ethanol solvent was removed under reduced pressure. A solution of NaOH (10.5 mmol) in 8.75 mL water was added to the residue, and the reaction mixture was heated under reflux (120 C) for 2 h. The reaction was subsequently cooled to room temperature and aqueous H2SO4 (15%) was added. The mercaptan separated as oil droplets and was extracted to diethylether (30 mL). The organic phase was washed twice with water, dried over anhydrous Na2SO4 and removed under reduced pressure. This yielded the desired mercaptans which were used without further purification for the synthesis of 1, 3 and 4.

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; Mostert, Samantha; Mentz, Wayne; Petzer, Anel; Bergh, Jacobus J.; Petzer, Jacobus P.; Bioorganic and Medicinal Chemistry; vol. 20; 24; (2012); p. 7040 – 7050;,
Bromide – Wikipedia,
bromide – Wiktionary

Share a compound : 40422-70-6

The synthetic route of 40422-70-6 has been constantly updated, and we look forward to future research findings.

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. 40422-70-6, name is 1-Bromo-3-(2-bromoethyl)benzene, A new synthetic method of this compound is introduced below., Product Details of 40422-70-6

To a 100 mL three neck round bottomed flask under nitrogen atmosphere, (R)-2- isopropyl-3,6-dimethoxy -2,5- dihydropyrazine (4 g, 21.7 mmol) was dissolved in dry THF (28 mL) and cooled to -78 C. To this reaction mixture, 1.6 M solution of n-BuLi in hexanes (16.28 mL, 26 mmol) was added dropwise at -78 C and stirred at same temperature for 15 minutes. After 15 minutes, l-bromo-3- (2-bromoethyl)benzene (5.73 g, 21.7 mmol) in dry THF (13 mL) was added dropwise at -78 C and stirred at -78 C for 1 h followed by stirring at room temperature (rt) for 3 h. The reaction was monitored by TLC using ethyl acctatc hcxancs (0.3:9.7) as a mobile phase. After completion of the reaction, reaction mixture was quenched with saturated ammonium chloride solution (75 mL) and extracted using ethyl acetate (3 x 100 mL). Combined organic layer was dried over sodium sulphate and concentrated to give crude which was purified by flash column purification with 1-3 % ethyl acetate in hexanes to yield 3.3 g of (2S,5R)-2-(3-bromophenethyl)-5- isopropyl-3, 6-dimethoxy-2,5-dihydropyrazine (41.38% yield).

The synthetic route of 40422-70-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PRINCIPIA BIOPHARMA INC.; LOU, Yan; OWENS, Timothy Duncan; BRAMELD, Kenneth Albert; GOLDSTEIN, David Michael; (171 pag.)WO2019/99576; (2019); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Discovery of 40422-70-6

The synthetic route of 40422-70-6 has been constantly updated, and we look forward to future research findings.

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. 40422-70-6, name is 1-Bromo-3-(2-bromoethyl)benzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1-Bromo-3-(2-bromoethyl)benzene

A mixture of 2,4,6-trimethyl-N-((3′-(methylsulfonyl)-[l, r-biphenyl]-4- yl)methyl)benzenesulfonamide (0.443 g, 1 mmol), K2CO3 (0.276 g, 2 mmol), and l-bromo-3-(2-bromoethyl)benzene (0.792 g, 3 mmol) in anhydrous acetonitrile (5 ml) was heated to 85 C for 2 h under microwave irradiation. The white powder was filtered off, the solvent was evaporated and the mixture was dissolved in ethyl acetate and extracted with brine. The organic phase was separated, dried over anhydrous MgS04, filtered and concentrated in vacuo. The remaining crude residue was purified by flash chromatography on silica gel (ethyl acetate/hexanes) to obtain the title compound as white sharp needles (88% based on recovery of the starting materials); FontWeight=”Bold” FontSize=”10″ H NMR (400 MHz, Chloroform-Patent; THE SCRIPPS RESEARCH INSTITUTE; KAMENECKA, Theodore, Mark; BURRIS, Thomas; WO2014/85453; (2014); A2;,
Bromide – Wikipedia,
bromide – Wiktionary