Category: 755027-18-0

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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-4-iodo-2-methoxybenzene

One-neck round bottom flask (One neck r.bf)on1-Bromo-4-iodo-2-methoxybenzene(50 g, 159.7 mmol),Triphenylene-2-ylboronic acid (500 mL / 100 mL), potassium carbonate (44.1 g, 319 mmol), 1,4-dioxane / water (43 mL), tetrakis (triphenylphosphine) palladium (0) (9.2 g, 7.89 mmol) The mixture was refluxed at 110 & lt; 0 & gt; C.Extraction with dichloromethane & lt; RTI ID = 0.0 & gt; MgS04 & lt; / RTI & gt;Filtered through silica gel and concentrated to give the compound 4-5-5. (48 g, 72%).

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; L Ti Material Co., Ltd.; Park Geon-yu; Noh Yeong-seok; Yang Seung-gyu; Cha Ju-hyeon; Kim Dong-jun; Choi Dae-hyeok; Lee Ju-dong; (100 pag.)KR2019/30963; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, belongs to iodides-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 755027-18-0, name: 1-Bromo-4-iodo-2-methoxybenzene

Step 4: l-Bromo-4-iodo-2-methoxybenzene (50 g, 160 mmol) was suspended in dichloromethane (75 mL) at -10 C. 1 N BBr3 in CH2Cl2 (250 mL, 250 mmol) was cannulated in over 30 minutes, with the internal temperature remaining below 0 C throughout the addition. After the addition, the mixture was stirred at 0C for 1 h, and then at room temperature for an additional 16 h. The mixture was cooled in an ice bath. 10% Aqueous Na2C03 (250 mL) was added in portions. The mixture was then partitioned between H20 and dichloromethane. The dichloromethane layer was dried over MgSCU and then filtered. 2-Bromo-5-iodophenol (46 g, 96%) was obtained from the filtrate as a pinkish- white solid. (1119) 1H NMR (acetone-< d: 9.24 (br s, 1H), 7.38 (d, J= 2 Hz, 1H), 7.31 (d, J= 8.5 Hz, 1H), 7.17 (dd, J= 8.5 Hz, 2 Hz, 1H). If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it. Reference:
Patent; PTC THERAPEUTICS, INC.; SYDORENKO, Nadiya; ALAM, Md Rauful; ARNOLD, Michael A.; BABU, Suresh; BHATTACHARYYA, Anuradha; CHEN, Guangming; GERASYUTO, Aleksey I.; KARP, Gary Mitchell; KASSICK, Andrew J.; MAZZOTTI, Anthony R.; MOON, Young-Choon; NARASIMHAN, Jana; PATEL, Jigar; TURPOFF, Anthony; WOLL, Matthew G.; YAN, Wuming; ZHANG, Nanjing; (0 pag.)WO2020/5873; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 755027-18-0, 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. 755027-18-0 name is 1-Bromo-4-iodo-2-methoxybenzene, 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.

General procedure: To a degassed solution of 1-bromo-4-iodo-2-methoxybenzene (2.2 g, 7.03 mmol), (4-methoxy-2-nitrophenyl)boronic acid (2.1 g, 10.55 mmol) in DME (80 mL) was added Pd(Ph3P)4 (812 mg, 0.7 mmol) and CsF (2.4 g, 15.82 mmol) under nitrogen. The reaction was then heated to 70 C for 18 h. The reaction was then extracted with EtOAc and water. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified silica (gradient elution, 3-40% EtOAc/hexanes) to give the title compound (2.7 g, 99%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-4-iodo-2-methoxybenzene, and friends who are interested can also refer to it.

Reference:
Article; Rudd, Michael T.; McCauley, John A.; Romano, Joseph J.; Butcher, John W.; Bush, Kimberly; McIntyre, Charles J.; Nguyen, Kevin T.; Gilbert, Kevin F.; Lyle, Terry A.; Holloway, M. Katharine; Wan, Bang-Lin; Vacca, Joseph P.; Summa, Vincenzo; Harper, Steven; Rowley, Michael; Carroll, Steven S.; Burlein, Christine; Dimuzio, Jillian M.; Gates, Adam; Graham, Donald J.; Huang, Qian; Ludmerer, Steven W.; McClain, Stephanie; McHale, Carolyn; Stahlhut, Mark; Fandozzi, Christine; Taylor, Anne; Trainor, Nicole; Olsen, David B.; Liverton, Nigel J.; Bioorganic and Medicinal Chemistry Letters; vol. 22; 23; (2012); p. 7201 – 7206;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 755027-18-0, These common heterocyclic compound, 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, 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.

A mixture of pyrazole-4-amine dihydrochloride (0.75 g, 4.79 mmol), salicylaldoxime (0.13115 g, 0.96 mmol), cesium carbonate (4.69 g, 14.38 mmol), cuprous oxide (0.06 g, 0.29 mmol), 1-bromo-4-iodo-2-methoxybenzene (1.5 g, 4.79 mmol) and N, N-dimethyl-formamide (5 ml) werecombined in a microwave vial fitted with an N2 inlet and magnetic stir bar. The reaction mixture wasstirred under a nitrogen atmosphere at 90 oc overnight. The solution obtained was allowed to coolto RT, then filtered through celite and the filtrate was concentrated in vacuo. The crude material20 was purified by silica gel chromatography (10% to 60% EtOAc in heptanes) to give 1-(4-bromo-3-methoxyphenyl)-1 H-pyrazol-4-amine (250 mg, MS: 270.2 [M+H+].)

Statistics shows that 1-Bromo-4-iodo-2-methoxybenzene is playing an increasingly important role. we look forward to future research findings about 755027-18-0.

Reference:
Patent; NOVARTIS AG; CHEUNG, Atwood; CHIN, Donovan Noel; DALES, Natalie; FAZAL, Aleem; HURLEY, Timothy Brian; KERRIGAN, John; O’BRIEN, Gary; SHU, Lei; SUN, Robert; SUNG, Moo; WO2014/28459; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, A new synthetic method of this compound is introduced below., Formula: C7H6BrIO

General procedure: A solution of the disulfide 5 (1.0 equiv) in anhydrous CH2Cl2was treated with TiCl4 (3.3 equiv) and subsequently MoCl5 (3.0equiv) or with MoCl3(HFIP)2 (3.0 equiv). Subsequently, a solutionof the aromatic compound (5.0 equiv) in anhydrous CH2Cl2was added dropwise,e and the mixture was stirred for the giventime (10-60 min) at r.t. at argon atmosphere. After completionof the reaction, a sat. aq solution of NaHCO3 was added and itwas stirred for additional 5 min. The mixture was extractedwith CH2Cl2, washed with brine, dried over MgSO4, and thesolvent was evaporated. The crude product was purified asdescribed below.

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; Franzmann, Peter; Beil, Sebastian B.; Winterscheid, Peter M.; Schollmeyer, Dieter; Waldvogel, Siegfried R.; Synlett; vol. 28; 8; (2017); p. 957 – 961;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 755027-18-0, A common heterocyclic compound, 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, molecular formula is C7H6BrIO, 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 a mixture of the product from Step 1, -bromo-4-iodo-2-methoxybenzene (750 mg, 2.4 mmol), CsF (1.09 g, 7.2 mmol), (2-amino-4-cyanophenyl)boronic acid hydrochloride (390 mg, 2.4 mmol), and Pd(PPh3)4 (277 mg, 0.24 mmol) was added DME (15 mL) under nitrogen. It was then heated to 100C. After 36 hours, EtOAc and water were added to the resulting thick red suspension. The organic layer was washed with brine, dried over Na2SO4, and the solvent was removed in vacuo. The residue was purified on silica (gradient EPO elution, 3-50% EtO Ac/hex anes) to yield the title compound as a red oil. LRMS (M+H)+ =303.1.

The synthetic route of 755027-18-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK & CO., INC.; WO2008/57208; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 755027-18-0, 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 755027-18-0 as follows.

in a sealable reaction tube was added i-brorno-4-iodo-2-rnethoxybenzene (2461 mg, 7.86 mrnol). tert-butyl I -oxo-2.8-diazaspiro[4.5] decane-8-carboxyiate (1000 mg, 3.93 mrnol), cesium carbonate (2562 mg, 7.86 rnrnol) and dioxane (7864 il). The reaction was purged with nitrogen. Then 9,9-dimethyi-4,5- bis(diphenyiphosphino)xanihene (341 rng, 0.590 mmol), Pd2(dba)3 (180 rng, 0.197 mrnoi)was added and nitrogen was bubbled through reaction for I mm. The reaction wassealed and stirred at 100 C overnight. The reaction was partitioned between EtOAc(50 ml) and water (30 ml). The organic layer was separated, washed with water (2 x 30m1) and brine (30 ml). dried over MgSO4, filtered and concentrated. The residue was purified using ISCO system (0-100% EtOAc/Hex gradient) to give tert-butyl 2-(4-bromo-3- rnethoxvphenyi)-i-oxo-2,8-diazaspiro[45]decane-8-carboxyiate (1.6 g, 364 mrnoi, 93 %yield) as a beige solid. ?H NMR (500MHz, DM50-do) d 7.67 (d, .J=2.2 Hz, 1H), 755(d, J=8.5 Hz, IH), 7.12 (dd, J=8.8, 2.5 Hz, 1H), 3.96 – 3.78 (m, 7H), 3.10 -2.84 (rn, 2H),2.10 (t. J=6.9 Hz, 21-1), 1.62 (dd, J=12.0, 4.0 Hz. 21-1), 1.51 (d, J=i3.5 Hz, 2F1), 1.42 (s,9H). MS (ESI) m/-: 43c.0, 441.0 (M+H).

According to the analysis of related databases, 755027-18-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ZHU, Yeheng; DEWNANI, Sunita, V.; EWING, William, R.; (265 pag.)WO2019/89868; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 755027-18-0, 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. 755027-18-0 name is 1-Bromo-4-iodo-2-methoxybenzene, 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.

General procedure: To a degassed solution of 1-bromo-4-iodo-2-methoxybenzene (2.2 g, 7.03 mmol), (4-methoxy-2-nitrophenyl)boronic acid (2.1 g, 10.55 mmol) in DME (80 mL) was added Pd(Ph3P)4 (812 mg, 0.7 mmol) and CsF (2.4 g, 15.82 mmol) under nitrogen. The reaction was then heated to 70 C for 18 h. The reaction was then extracted with EtOAc and water. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified silica (gradient elution, 3-40% EtOAc/hexanes) to give the title compound (2.7 g, 99%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-4-iodo-2-methoxybenzene, and friends who are interested can also refer to it.

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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, A new synthetic method of this compound is introduced below., Formula: C7H6BrIO

To a solution of 2-bromo-5-iodoanisole (12.5 g, 40 mmol) in DCM (200 mL) was added a 1.0 M DCM solution OfBBr3 (40 mL) dropwise at 0 0C. The reaction mixture was then allowed to warm to room temperature. After stirring overnight, the reaction mixture was cooled to 0 C and MeOH (5 mL) was added dropwise. After stirring for 10 minutes at room temperature, the reaction mixture was washed with IN HCl (2 x 50 mL), water (50 mL) and brine (50 mL). The organic layer was dried over MgSO4. filtered and concentrated under vacuum. The residue was then dissolved in DMF (100 mL) and Cs2CO3 (26 g, 80 mmol) and 2-(benzyloxycarbonylamino)ethyl methanesulfonate (11 g, 40 mmol) were added. After stirring at 80C under nitrogen for 4 h, the reaction mixture was dissolved in EtOAc (100 mL). The organic layer was washed with brine (3 x 50 mL), dried over MgSO4 and filtered. The solvent was removed under vacuum and the crude compound was purified by flash chromatography using cyclohexane/EtOAc (85/15) as eluent to afford the title compound (11.5 g, 60% yield) as a white solid. ESMS; m/z 476, 478 (M+l), 493, 495 (M+18) 1H-NMR (CDCl3): 53.64 (q, J= 5.2 Hz, 2H), 4.05 (t, J= 4.7 Hz, 2H), 5.12 (s, 2H), 5.33 (bs, IH), 7.15-7.24 (m, 3H), 7.35 (bs, 5H).13C-NMR (CDCl3): 540.4, 67.0, 68.7, 92.4, 112.4, 122.7, 128.2, 128.2, 128.6, 131.5, 134.6, 136.4, 155.4, 156.4.Theoretical Mass: (M + Na) 497.91777. Measured Mass: (M + Na) 497.91638 Microanalysis: %C 40.41 (40.36), %H 3.24 (3.18), %N 2.86 (2.94) M.p. 700C

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; UCL BUSINESS PLC; WO2009/27679; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 1-Bromo-4-iodo-2-methoxybenzene

A solution of 1-bromo-4-iodo-2-methoxybenzene (0.63 g, 2.01 mmol) dissolved in toluene (15.7 mL) was treated with 2-methoxy-N-methylethanamine (179 mg, 2.01 mmol), sodium tert-butoxide (232 mg, 2.42 mmol), Xantphos (0.116 g, 0.20 mmol) and tris(dibenzylideneacetaone)dipalladium (0) (46 mg, 0.05 mmol) under a nitrogen atmosphere. The resulting mixture was stirred at 80 C in a sealed tube for 2 hours. The reaction mixture was diluted with water (200 mL), and extracted with EtOAc (200 mL). The organic layerwas dried over MgSO4, filtered and evaporated to afford the crude product. The crudeproduct was purified by flash silica chromatography eluting with 50% Et2O in heptane. Purefractions were evaporated to dryness to afford 4-bromo-3-methoxy-N-(2-methoxyethyl)-Nmethylaniline(231 mg, 42%) as a brown solid.

The synthetic route of 755027-18-0 has been constantly updated, and we look forward to future research findings.