Category: 26670-89-3

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. 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 2-Bromo-4-iodo-1-methylbenzene

Compound 1 (3 g, 10.10 mmol, 1 eq) in THF (30 mL) was placed into 250 ml round bottom flask. The reaction solution was cooled to -65 C. under a nitrogen atmosphere. n-BuLi (2.2 M, 5.05 mL, 1.1 eq) to the cooled solution was slowly added dropwise, the mixture was stirred for 1 h at the same temperature. TRIMETHYL BORATE (1.26 g, 12.12 mmol, 1.37 mL, 1.2 eq) were added dropwise to the above solution at the same temperature. The mixture was stirred at -65 OC for 1 h. Then cool bath was removed and the mixture was stirred at -65?10 C. for 16 h. The mixture was acidified by dropwise addition of HCl solution (2 M, 5 mL) to the reaction solution, which was stirred for 1.5 hour. The mixture were concentrated in vacuum to afford a residue. The residue was purified by reverse-MPLC (FA condition, A: water, B: MeCN, 40% B). The fraction were concentrated to remove solvent, and aqueous phase was extracted with ethyl acetate (50 mL*3). The combined organic layers were washed with brine (50 mL), dried over sodium sulfate, filtered and the filtrate was concentrated in vacuum to give Compound 2 (1.3 g, 6.05 mmol, 59% yield) as white solid. 1H NMR (400 MHz, DMSO-d6) delta=8.15 (s, 0.5H), 7.95 (s, 0.3H), 7.93 (s, 1H), 7.73 (d, J=7.5 Hz, 1H), 7.66 (d, J=7.5 Hz, 0.3H), 7.37 (d, J=7.5 Hz, 1H), 7.32 (d, J=7.6 Hz, 0.3H), 2.37 (s, 3H), 2.34 (s, 0.9H).

The synthetic route of 26670-89-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; 1ST Biotherapeutics, Inc.; LEE, Jinhwa; KIM, Jae Eun; JO, Suyeon; LEE, Gwibin; LIM, Keonseung; PARK, A Yeong; KIM, Misoon; JUNG, Gyooseung; LIM, Seung Mook; LEE, Minwoo; YANG, Heekyoung; KIM, Hyonam; KIM, Hyeongjun; LI, Wanjun; FAN, Mingzhu; (82 pag.)US2019/100500; (2019); 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. 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 26670-89-3

Compound 1 (3 g, 10.10 mmol, 1 eq) in THF (30 mL) was placed into 250 ml round bottom flask. The reaction solution was cooled to -65 C. under a nitrogen atmosphere. n-BuLi (2.2 M, 5.05 mL, 1.1 eq) to the cooled solution was slowly added dropwise, the mixture was stirred for 1 h at the same temperature. TRIMETHYL BORATE (1.26 g, 12.12 mmol, 1.37 mL, 1.2 eq) were added dropwise to the above solution at the same temperature. The mixture was stirred at -65 OC for 1 h. Then cool bath was removed and the mixture was stirred at -65?10 C. for 16 h. The mixture was acidified by dropwise addition of HCl solution (2 M, 5 mL) to the reaction solution, which was stirred for 1.5 hour. The mixture were concentrated in vacuum to afford a residue. The residue was purified by reverse-MPLC (FA condition, A: water, B: MeCN, 40% B). The fraction were concentrated to remove solvent, and aqueous phase was extracted with ethyl acetate (50 mL*3). The combined organic layers were washed with brine (50 mL), dried over sodium sulfate, filtered and the filtrate was concentrated in vacuum to give Compound 2 (1.3 g, 6.05 mmol, 59% yield) as white solid. 1H NMR (400 MHz, DMSO-d6) delta=8.15 (s, 0.5H), 7.95 (s, 0.3H), 7.93 (s, 1H), 7.73 (d, J=7.5 Hz, 1H), 7.66 (d, J=7.5 Hz, 0.3H), 7.37 (d, J=7.5 Hz, 1H), 7.32 (d, J=7.6 Hz, 0.3H), 2.37 (s, 3H), 2.34 (s, 0.9H).

The synthetic route of 26670-89-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; 1ST Biotherapeutics, Inc.; LEE, Jinhwa; KIM, Jae Eun; JO, Suyeon; LEE, Gwibin; LIM, Keonseung; PARK, A Yeong; KIM, Misoon; JUNG, Gyooseung; LIM, Seung Mook; LEE, Minwoo; YANG, Heekyoung; KIM, Hyonam; KIM, Hyeongjun; LI, Wanjun; FAN, Mingzhu; (82 pag.)US2019/100500; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 26670-89-3,Some common heterocyclic compound, 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, molecular formula is C7H6BrI, 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.

(2-2) Synthesis of 2-Bromo-1-Methyl-4-Phenylbenzene (0144) A mixture of 2-bromo-4-iodotoluene (14.5 g) obtained by the step (2-1), phenylboronic acid (6.35 g), tetrakis(triphenylphosphine)palladium (0) (1.69 g), potassium carbonate (20.2 g), 1,4-dioxane (117 mL), and water (13 mL) was refluxed for 3 hours in an argon atmosphere. The resulting reaction mixture was returned to room temperature, and extracted with dichloromethane. The organic layer was washed with a saturated sodium chloride solution, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 2-bromo-1-methyl-4-phenylbenzene (8.6 g). The yield was 71%.

The synthetic route of 26670-89-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IDEMITSU KOSAN CO., LTD.; ITO, Hirokatsu; KAWAMURA, Masahiro; MIZUKI, Yumiko; HAKETA, Tasuku; HAYAMA, Tomoharu; TAKAHASHI, Ryota; (141 pag.)US2017/183291; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 26670-89-3,Some common heterocyclic compound, 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, molecular formula is C7H6BrI, 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.

In a 1 L four-necked round bottom flask equipped with a stirrer, Erlin condenser, nitrogen inlet tube, and thermometer, 19.3 g (91.0 mmol) of 4-dibenzofuran boronic acid of Synthesis Example 8, 2 (100.0 mmol) of bromo-4-iodotoluene, 300 mL of toluene, 150 mL of ethanol, 25.1 g (181.5 mmol) of potassium carbonate and 90 mL of water, and the mixture was stirred at room temperature for 30 minutes under a nitrogen stream. Subsequently, 0.10 g (0.45 mmol) of palladium acetate and 0.27 g (0.91 mmol) of tri (o-tolyl) phosphine were added and heated, followed by stirring at a reflux temperature for 2 hours. The resulting reaction solution was cooled to room temperature, the aqueous layer was separated, and extracted twice with 100 mL of ethyl acetate. Next, the organic layers were combined, washed with 100 mL of saturated brine, dried over magnesium sulfate, magnesium sulfate was removed by suction filtration, and the solvent was distilled off under reduced pressure. Subsequently, the obtained oily matter was separated by silica gel column chromatography with a mixed solvent of n-heptane and toluene to obtain 23.3 g (yield: 75.9%) of the desired bromide.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-4-iodo-1-methylbenzene, its application will become more common.

Related Products of 26670-89-3,Some common heterocyclic compound, 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, molecular formula is C7H6BrI, 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.

In a 100 mE round-bottomed flask under argon, 1 g of 2-bromo-4-iodoroluene (3.37 mmol; 1 eq) and 0.51 g methyl azetidine-3-carboxylate, hydrochloride (preparation 1; 3.36 mmol; 1 eq) were dissolved in 10 mE of toluene. The solution was degassed with argon 4.39 g of cesium carbonate (13.47 mmol; 4 eq) 62mg of Pd2(dba)3 (0.07 mmol; 0.02 eq). and 117 g of Xant-Phos (0.20 mmol; 0.06 eq) were successively added and the reaction medium was stirred at 100 C. overnight. It was brought back to RT and diluted in EtOAc, then washed with watet The aqueous phase was extracted once again with EtOAc. The combined organic phases were dried over MgSO4, filtered and evaporated to give 1.15 g of a colorless oil. It was purified by flash chromatography on silica using a cyclohexane/0% to 10% EtOAc gradient, to give 510mg of the title compound in the form of a brown oil.Yld: 53%.?H NMR (300 MHz, DMSO-d5) oeppm 2.21 (s, 3H); 3.55-3.70 (m, 1H); 3.67 (s, 3H); 3.84-3.87 (m, 2H);3.97-4.03 (m, 2H); 6.39 (dd, J=8.4, 2.4 Hz, 1H); 6.65 (d, J=2.4 Hz, 1H); 7.13 (d, J=8.4 Hz, 1H).11015] LC-MS: m/z (M+H): 284.

The synthetic route of 26670-89-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INVENTIVA; BOUBIA, Benaissa; MASSARDIER, Christine; GUILLIER, Fabrice; POUPARDIN, Olivia; TALLANDIER, Mireille; AMAUDRUT, Jerome; BONDOUX, Michel; FEENSTRA, Roelof Williem; VAN DONGEN, Maria Johana Petronella; (207 pag.)US2017/66717; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 2-Bromo-4-iodo-1-methylbenzene

7H-pyrrolo[2,3-d]pyrimidin-2-amine (134 mg, 1.00 mmol), 2-bromo-4-iodo-1-toluene (600 mg, 2.00 mmol),potassium carbonate (415 mg, 3.00 mmol) and proline (23 mg, 0.2 mmol) was added to the eggplant flask,dimethyl sulfoxide was added, and the reaction solution was deoxidized. Copper iodide (19 mg, 0.1 mmol) was added and the reaction solution was deoxygenated. Heat to 90 C and stir for 16 hours. After the reaction was completed, it was cooled to room temperature, water and ethyl acetate were added, and the mixture was filtered over celite. The target compound was obtained in an amount of 200 mg.

According to the analysis of related databases, 26670-89-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Chinese Academy Of Sciences Shanghai Pharmaceutical Institute; Zhao Yujun; Li Zhiqiang; Yan Ziqin; Li Jia; Zhou Yubo; Su Mingbo; Chen Zheng; (138 pag.)CN109810110; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 26670-89-3, 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. 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

2,6-Difluoro-N-(2′-methyl-5′-(pyridin-3-ylethynyl)biphenyl-4-yl)benzamide[00148] To the solution of 2-bromo-4-iodo-l-methylbenzene (0.3 g, 1.0 mmol) in TEA (4 mL) and toluene (1 mL) was added 3-ethynylpyridine (0.115 g, 1.12 mmol), CuI (0.04 g, 0.2 mmol), and Pd(PPh3)4 (0.065 g, 0.06 mmol). The resulting solution was heated at 1000C overnight before it was diluted with water and extracted with EtOAc (3chi20mL). The combined organic phases were dried and concentrated, and the column chromatography (Hexanes/EtOAc=l/l) afforded 2 in 66% yield. The desired compound was obtained from 2 through Suzuki coupling.[00149] 1H NMR (400 MHz, CDCb) delta 8.75 (d, / = 1.2 Hz, 1 H), 8.54-8.52 (m, 1 H), 7.81-7.78 (m, 1 H), 7.72-7.68 (m, 3 H), 7.45-7.43 (m, 3 H), 7.37-7.34 (m, 2 H), 7.29-7.27 (m, 2 H), 7.03 (t, / = 8.0 Hz, 2 H), 2.31 (s, 3 H); ESMS cacld (C27H18F2N2O): 424.1; found: 425.1 (M+H).

The chemical industry reduces the impact on the environment during synthesis 2-Bromo-4-iodo-1-methylbenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SYNTA PHARMACEUTICALS CORP.; JIANG, Jun; ZHANG, Junyi; CHEN, Shoujun; SUN, Lijun; WO2010/39238; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com