Month: March 2021

Related Products of 175278-30-5, 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. 175278-30-5, name is 4-Bromo-2-ethyl-1-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

First, 65 g (209 mmol) of 1-iodo-2-ethyl-4-bromobenzene and 38 g (226 mmol) of 4-n-butylphenylacetylene were introduced into 300 ml of NEt3, 1 g (5.3 mmol) of copper (I) iodide 3.6 g (5.1 mmol) bis (triphenylphosphine) palladium (II) chloride, and the mixture was stirred at room temperature for 2 hours. The batch was cooled, water and heptane were added, and the phases were separated. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated on a rotary evaporator. The residue was purified by column chromatography (SiO2, heptane); the product was obtained as a colorless oil.

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, 4-Bromo-2-ethyl-1-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK PATENT GMBH; JASPER, CHRISTIAN; BROCKE, CONSTANZE; PAULUTH, DETLEF; REIFFENRATH, VOLKER; MANABE, ATSUTAKA; (37 pag.)TW2017/16378; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 3032-81-3, 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. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows.

To a stirred solution of l,3-dichloro-5-iodobenzene (4.0 g, 14.6 mmol) in THF (30 mL), LDA (2.0 M in THF/heptane/ethylbenzene, 9.6 mL, 16.9 mmol) was added dropwise at -78 ¡ãC and stirred for 1 h at the same temperature. A solution of DMF (1.7 mL, 22.0 mmol) in THF (5 mL) was added slowly at -78 ¡ãC and stirred for 3 h. The reaction mixture was quenched with saturated NH4C1 (50 mL) and extracted with EtOAc (2 x 30 mL). The combined organic layers were washed with water (50 mL), brine (50 mL), dried over anhydrous Na2S04 and concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel, 20percent EtOAc/hexane as eluent) to afford compound A35-1 (1.4 g, 32percent) as colorless oil.

The chemical industry reduces the impact on the environment during synthesis 1,3-Dichloro-5-iodobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; TEIJIN PHARMA LIMITED; AMGEN INC.; BECK, Hilary Plake; BOOKER, Shon Keith; BREGMAN, Howard; CEE, Victor J.; CHAKKA, Nagasree; CUSHING, Timothy D.; EPSTEIN, Oleg; FOX, Brian M.; GEUNS-MEYER, Stephanie; HAO, Xiaolin; HIBIYA, Kenta; HIRATA, Jun; HUA, Zihao; HUMAN, Jason; KAKUDA, Shinji; LOPEZ, Patricia; NAKAJIMA, Ryota; OKADA, Kazuhisa; OLSON, Steven H.; OONO, Hiroyuki; PENNINGTON, Lewis D.; SASAKI, Kosuke; SHIMADA, Keiko; SHIN, Youngsook; WHITE, Ryan D.; WURZ, Ryan P.; YI, Shuyan; ZHENG, Xiao Mei; WO2015/129926; (2015); 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. 116632-39-4, name is 5-Bromo-2-iodotoluene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H6BrI

4-bromo-1-iodo-2-methylbenzene (31.2 g, 105 mmol), (2-(methoxycarbonyl)phenyl)boronic acid (24.5 g, 136 mmol), Pd(dppf)Cl2 (2.3 g, 3.15 mmol) and potassium carbonate (72.5 g, 525 mmol) were added to 350 mL of toluene in a 1 L three-neck round bottom flask. The resulting mixture was purged with nitrogen for 5 min and refluxed overnight under nitrogen. After cooling to room temperature, the reaction mixture was filtered through Celite and washed with ethyl acetate. The organic extract was dried over anhydrous Na2SO4 and concentrated. The residue was purified by flash column chromatography (eluent: ethyl acetate/petroleum ether=1/100, v/v) to give methyl 4′-bromo-2′-methyl-[1,1′-biphenyl]-2-carboxylate as a light yellow oil (20 g, 62%).

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 116632-39-4.

Reference:
Patent; Xia, Chuanjun; (88 pag.)US2019/127406; (2019); 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. 116632-39-4, name is 5-Bromo-2-iodotoluene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 116632-39-4

Preparation 9 2-(2-Bromo-5-iodo-4-methylbenzyl) isoindoline-1,3-dione To a solution of 5-bromo-2-iodo toluene (512 mg, 1.72 mmol) in trifluoroacetic acid (5 mL) was added N-(hydroxymethy) phthalimide (305 mg, 1.72 mmol). The mixture developed a pink color. The solution was stirred at room temperature for 22 hours then concentrated sulfuric acid (1 mL) was added. The homogeneous solution was stirred for 18 hours at room temperature. Water was added and the precipitated solid collected by filtration and dried in a current of air (0.776 gm). This material, which by proton NMR analysis contained approximately 15% of an isomeric product, was carried forward to the following procedure without further purification. 1H NMR (400 MHz, CDCl3) delta7.85 (m, 2H) 7.76(m, 2H) 7.5 (s, 1H) 7.38(s, 1H) 4.84(s, 2H) 2.31(s, 3H). GC-MS calc. 455, found 455.

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 116632-39-4.

Reference:
Patent; Pfizer Inc; US2007/213371; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 21740-00-1, name is 5-Bromo-2-iodobenzoic acid, 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 21740-00-1, Application In Synthesis of 5-Bromo-2-iodobenzoic acid

Concentrated H2S04 (10 mL) was added dropwise to the solution of 5- bromo-2-iodobenzoic acid (100 g, 305.89 mmol) in MeOH (800 mL). The mixture was refluxed for 16 hours and then concentrated. The residue was dissolved in ethyl acetate (1 L). The organic layer was washed with saturated NaHCO3 and brine (3 x 200 mL), dried over Na2SO4, filtered and concentrated to afford targetproduct 5-Bromo-2-iodo-benzoic acid methyl ester (101.4 g, yield 90%) as yellow solid.LC purity: 98.91 % (254 nm); Mass: find peak 341 (M + H)+ at 2.214 mm.

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; SANOFI; PASCAL, Cecile; PELLET, Alain; COURTEMANCHE, Gilles; CAMPBELL, Simon; (78 pag.)WO2019/8027; (2019); 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. 10297-05-9, name is 1-Chloro-4-iodobutane, This compound has unique chemical properties. The synthetic route is as follows., category: iodides-buliding-blocks

(1) Preparation of 1-(4-chlorobutoxy)-4-iodobenzene To a solution of 4-iodophenol (1.0 g) in acetonitrile (10 mL), cesium carbonate (3.0 g) and 1-chloro-4-iodobutane (1.2 g) were added and the mixture was heated to 100¡ãC, at which it was stirred for 4 hours. The reaction mixture was cooled to room temperature and filtered to remove insoluble materials, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by NH-type silica gel column chromatography (eluding solvent: n-hexane:ethyl acetate = 7:3 to 1:1) to give the titled compound (1.4 g, 99percent) as a brown oil.

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 10297-05-9.

Reference:
Patent; TAISHO PHARMACEUTICAL CO., LTD; EP2221298; (2010); 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. 13194-68-8, name is 4-Iodo-2-methylaniline, A new synthetic method of this compound is introduced below., Quality Control of 4-Iodo-2-methylaniline

(a) Preparation of 4-Fluoro-2-(4-iodo-2-methyl-phenylamino)-benzoic acid To a stirred solution containing 3.16 g (0.0133 mol) of 2-amino-5-iodotoluene in 5 mL of tetrahydrofuran at -78 C. was added 10 mL (0.020 mol) of a 2.0 M lithium diisopropylamide in tetrahydrofuran/heptane/ethylbenzene (Aldrich) solution. The resulting green suspension was stirred vigorously for 15 minutes, after which time a solution of 1.00 g (0.00632 mol) of 2,4-difluorobenzoic acid in 10 mL of tetrahydrofuran was added. The reaction temperature was allowed to increase slowly to room temperature, at which temperature the mixture was stirred for 2 days. The reaction mixture was concentrated by evaporation of the solvent under reduced pressure. Aqueous HCl (10%) was added to the concentrate, and the solution was extracted with dichloromethane. The organic phase was dried (MgSO4) and then concentrated over a steambath to low volume (10 mL) and cooled to room temperature. The off-white fibers which formed were collected by vacuum filtration, rinsed with hexane, and dried in a vacuum-oven (76 C.; ca. 10 mm of Hg) to afford 1.10 g (47%) of the desired material; mp 224-229.5 C.; 1H NMR (400 MHz, DMSO): delta 9.72 (s, 1H), 7.97 (dd, 1H, J=7.0, 8.7 Hz), 7.70 (d, 1H, J=1.5 Hz), 7.57 (dd, 1H, J=8.4, 1.9 Hz), 7.17 (d, 1H, J=8.2 Hz), 6.61-6.53 (m, 2H), 2.18 (s, 3H); 13C NMR (100 MHz, DMSO): delta 169.87, 166.36 (d,JC-F=249.4 Hz), 150.11 (d, JC-F=11.4 Hz), 139.83, 138.49, 136.07, 135.26 (d,JC-F=11.5 Hz), 135.07, 125.60, 109.32, 104.98 (d, JC-F=21.1 Hz), 99.54 (d, JC-F=26.0 Hz), 89.43, 17.52; 19F NMR (376 MHz, DMSO): delta-104.00 to -104.07 (m); IR (KBr) 1670 (C=O stretch)cm-1; MS (CI) M+1=372. Analysis calculated for C14H11FINO2: C, 45.31; H, 2.99; N, 3.77. Found: C, 45.21; H, 2.77; N, 3.64.

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; Gowan, Richard Carleton; Sebolt-Leopold, Judith; US2004/171632; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 16355-92-3,Some common heterocyclic compound, 16355-92-3, name is 1,10-Diiododecane, molecular formula is C10H20I2, 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′-(4S,4’S)-8,8′-(decane-1,10-diylbis(oxy)bis(6-(4-chlorophenyl)-1-methyl- 4H-benzo[f][1,2,4]triazolo[4,3-a][1,4]diazepine-8,4-diyl))bis(N-ethylacetamide) [Example 11]: A suspension of 2-(4S)-6-(4-chlorophenyl)-8-hydroxy-1-methyl-4H- benzo[f][1,2,4]triazolo[4,3-a][1,4]diazepin-4-yl)-N-ethylacetamide (208 mg, 0.507 mmol) in acetonitrile (10 mL) was charged with K2CO3 (82 mg, 0.6 mmol) and 1,10-diiododecane (100 mg, 0.254 mmol) and the resulting mixture was heated at 80 oC for 12 h. After the completion of reaction, the reaction mixture was concentrated in vacuo and the residue was partitioned between DCM (20 mL) and H2O (10 mL) and separated. The aqueous layer was re-extracted with DCM (3 X 15 mL) and the combined organic fractions were dried over anhydrous Na2SO4, filtered and concentrated in vacuo resulting in a crude product which was purified by preparative HPLC to afford 30 mg, (12 % yield ) of the title compound as a white solid. 1H NMR (400 MHz, DMSO-d6): = 8.26- 8.15 (m, 2H), 7.78 (t, J = 8.8 Hz, 2H), 7.50- 7.31 (m, 10H), 6.89- 6.80 (m, 2H), 4.47- 4.40 (m, 2H) , 4.06 – 3.85 (m, 4H), 3.36- 3.05 (m, 8H), 2.52 (s, 6H), 1.80- 1.60 (m, 4H), 1.40- 1.21 (m, 12H), 1.06 (t, J = 7.2 Hz, 6H); MS (ES+): m/z = 958.65, 960.70 [M+H] +; LCMS: tR = 3.3 min.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,10-Diiododecane, its application will become more common.

Reference:
Patent; COFERON, INC.; ARNOLD, Lee, Daniel; FOREMAN, Kenneth, W.; JIN, Meizhong; WANNER, Jutta; WERNER, Douglas, S.; WO2015/81284; (2015); 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. 5471-81-8, name is Methyl 4-iodo-3-methylbenzoate, This compound has unique chemical properties. The synthetic route is as follows., category: iodides-buliding-blocks

0.2 mmol of cesium carbonate, 0.01 mmol of palladium acetate, 0.02 mmol of triphenylphosphine,1,4-Dihydro-1,4-epoxy naphthalene 0.2 mmol, methyl 4-iodo-3-methylbenzoate 0.1 mmol,0.15 mmol of hexamethyldisilazide and 1 ml of N,N-dimethylformamide were added to a 15 ml reaction tube.Nitrogen was repeatedly filled 3 times, placed in an oil bath at 100 C, reacted for 12 h; cooled to room temperature,The reaction solution was diluted with ethyl acetate and washed with water three times.The organic phase is dried over anhydrous Na2SO4.Filtered, concentrated, and purified by column chromatography36.3 mg of target product, yield 83%

According to the analysis of related databases, 5471-81-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (13 pag.)CN108586519; (2018); A;,
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. 56404-21-8, name is 1-Iodo-2,4-dimethyl-3-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C8H8INO2

A mixture of l-iodo-2,4-dimethyl-3-nitrobenzene [56404-21-8] (1.50 g, 5.41 mmol), methyl 2,2-difluoro-2-(fluorosulfonyl)acetate [680-15-9] (6.24 g, 32.5 mmol), Cul (1.24 g, 6.50 mmol) and DIPEA (0.70 g, 5.41 mmol) in anhydrous DMF (13.9 mL) was stirred at 80 C for 2 h. The mixture was poured out in water and the aqueous phase was extracted with Et20. The combined organic extracts were washed with brine, dried (MgS04), filtered and concentrated under reduced pressure. The crude mixture was purified by flash column chromatography (silica, pentane/Et20, gradient from 100:0 to 90:10) to afford I- 100 (840 mg, 71%) as a yellow oil.

The synthetic route of 56404-21-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BARTOLOME-NEBREDA, Jose Manuel; TRABANCO-SUAREZ, Andres, Avelino; LEENAERTS, Joseph, Elisabeth; OEHLRICH, Daniel; BUIJNSTERS, Peter Jacobus Johannes Antonius; MARTINEZ LAMENCA, Carolina; VELTER, Adriana, Ingrid; VAN ROOSBROECK, Yves, Emiel, Maria; (110 pag.)WO2019/243533; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com