Tag: M.W=300-400

Application of 811842-30-5, 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. 811842-30-5, name is 2-Bromo-1-fluoro-4-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows.

Preparation 13 2-(3-Bromo-4-fluorophenyl)-4,4,5,5-tetramethyl-1 ,3,2-dioxaborolane To a mixture of 2-bromo-1-fluoro-4-iodobenzene (5.0 g, 16.62 mmo) in dioxane (75 mL) was added bis(pinacolato)diboron (4.2 g, 16.62 mmol) and potassium carbonate (3.3 g, 33.2 mmol). The mixture was degassed and recharged with nitrogen. Bis(triphenylphosphine)palladium(ll)dichloride (0.60 g, 0.83 mmol) was added and the mixture heated to 100C for 18 hours under a nitrogen atmosphere. The mixture was diluted with ethyl acetate (300 mL) and washed with saturated ammonium chloride solution, water and brine (200 mL each). The organic layer was evaporated to give the title compound as dark red oil (6.1 g) which was used without further purification. 1 H NMR (400 MHz, CDCI3): delta ppm 1 .33 (s, 12H), 7.10 (t, 1 H), 7.72-7.65 (m, 1 H), 8.00 (dd, 1 H) ppm.

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

Reference:
Patent; PFIZER LIMITED; OWEN, Robert Mckenzie; PRYDE, David Cameron; TAKEUCHI, Mifune; WATSON, Christine Anne Louise; WO2015/189744; (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. 755027-18-0, name is 1-Bromo-4-iodo-2-methoxybenzene, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 1-Bromo-4-iodo-2-methoxybenzene

Compound 135 (2.00 g, 6.39 mmol) and Compound 170 (2.174 g, 7.03 mmol) were dissolved in 1,4-dioxane (20 ml), to which were then added tetrakis(triphenylphosphine)palladium (0.739 g, 0.639 mmol) and 2 mol/L aqueous solution of potassium carbonate (4.79 ml, 9.59 mmol), and the reaction mixture was stirred at 100C. After completion of the reaction, chloroform and water were added to the reaction mixture, and the resulting mixture was filtered. The obtained filtrate was extracted with chloroform. The obtained organic layer was dried over magnesium sulfate, and then the solvent was removed by concentration under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain Compound 171.

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; Shionogi & Co., Ltd.; TAMURA, Yuusuke; HINATA, Yu; KOJIMA, Eiichi; OZASA, Hiroki; (241 pag.)EP3187498; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 689291-89-2, name is 5-Bromo-2-iodobenzaldehyde, 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 689291-89-2, COA of Formula: C7H4BrIO

(Z)-l,2-bis(5-bromo-2-iodophenyl)ethene (18a). A solution of phosphonium salt 16a (3.84 g, 6.02 mmol) in THF (60 mL) was cooled to 0 C in a 250 mL Schlenk flask under nitrogen with stirring. Potassium ‘butoxide (815 mg, 7.12 mmol) was added portionwise and the resulting mixture was held at 0 C for 30 min. A solution of benzaldehyde 17a (1.7 g, 5.5 mmol) in THF (60 mL) was added dropwise at 0 C and the reaction was allowed to warm up to room temperature and left stirring for 24 h. The reaction mix was partitioned between 1 : 1 water: diethyl ether. The aqueous layer was removed and extracted with diethyl ether (3x) and the organics were dried with MgS04, filtered and the solvent removed under reduced pressure to provide an off white solid that was further purified by a short plug (Si02: 10% ethyl acetate in hexane) to yield 2.95 g (4.99 mmol, 91%) 82:18 Z:E of 18a as an off-white solid that was used without further purification. -NMR (400 MHz, CDC13) delta: 7.70 (d, 2H, J= 8.4 Hz), 7.05 (dd, 2H, J= 8.4, 2.4 Hz), 7.02 (d, 2H, J= 2.4 Hz), 6.58 (s, 2H); HRMS (FAB) m/z calculated for Ci4H8Br2l2 Pv ]; 587.7082, found 587.7067.

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, 5-Bromo-2-iodobenzaldehyde, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE JOHNS HOPKINS UNIVERSITY; TOVAR, John Dayton; CARUSO, Jr., Anthony; WO2011/127383; (2011); A2;,
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. 51560-21-5, name is 1,4-Diiodo-2,5-dimethoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 51560-21-5

Example 3.3; Synthesis of 2,5-diiodo- 1 ,4-hydroquinone; A solution of 2,5-diiodo- 1,4-dimethoxybenzene (3.0Og, 7.69 mmol) in 30 ml ofAnhydrous dichloromethane was cooled to -80C and BBr3 (19 ml, 16.93 mmol) was added drop wise. The mixture was allowed to rt and stirred for additional 12h, solid precipitate was formed, collected and then crystallized from ethanol-water. The trace of solvent was evaporated at reduced pressure(2.50 g, yield 90 %).

The synthetic route of 51560-21-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITA’ DEGLI STUDI DI BARI; CONSIGLIO NAZIONALE DELLE RICERCHE; UNIVERSITA’DEGLI STUDI DEL SALENTO; WO2008/96239; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 181765-86-6, 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 181765-86-6 as follows.

To a solution of 5-Bromo-2-iodo-benzoic acid methyl ester (24 g, 70.4 mmol) and methyl 2,2-difluoro-2- (fluorosulfonyl)acetate (13.5 mL, 105.6 mmol) inN-methyl-2-pyrrolidinone (80 mL) was added copper (I) bromide (1.21 g, 8.45 mmol). The reaction mixture was stirred at 100C for 5 hours. The reaction was filtered and partitioned between ethyl acetate and brine. The aqueous layer was extracted with ethyl acetate, and the organic layers were combined and dried over Na2SO4. After filtration, the solvent was removed in vacuo. The residue waspurified by silica gel column (0-4% Ethyl acetate in Petroleum ether) to give the 5-Bromo-2-trifluoromethyl-benzoic acid methyl ester (119.2 g, yield 96%) as yellow oil.

According to the analysis of related databases, 181765-86-6, the application of this compound in the production field has become more and more popular.

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

Adding a certain compound to certain chemical reactions, such as: 400-97-5, name is 1-Iodo-2-nitro-4-(trifluoromethyl)benzene, 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 400-97-5, Recommanded Product: 400-97-5

b Preparation of 2-amino-4-trifluoromethyliodobenzene: A mixture of 225 ml of water, 166 g of iron and 10.03 g of ammonium chloride are heated to reflux. 317 g of 2-nitro-4-trifluoromethyliodobenzene are added thereto over a period of 2 hours, then refluxing is continued for 3 hours 30 minutes when the addition is complete. The whole is allowed to cool then the medium is extracted 4 times with 250 ml of benzene each time. The mixture is then filtered and subsequently decanted. The organic layer is dried and the solvent is evaporated. After distillation, 256 g of 2-amino-4-trifluoromethyliodobenzene are recovered, b.p.: 102 to 114 C., ind (25 C.): 1.556. (Yield: 89.5%).

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; Adir et Compagnie; US5079245; (1992); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 54507-44-7,Some common heterocyclic compound, 54507-44-7, name is 2-Iodo-4-(trifluoromethyl)benzoic acid, molecular formula is C8H4F3IO2, 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.

Intermediate AI: S-trifluoromethyl-biphenyM-carboxylic acidA mixture of 2-iodo-4-trifluoromethyl-benzoic acid (CAS: 54507-44-7) (300 mg, 0.949 mmol) phenylboronic acid (239 mg, 1.898 mmol), sodium carbonate (302 mg, 2.847 mmol) and palladium (II) acetate (10.7 mg, 0.0475 mmol) in 4.5 ml water was stirred at room temperature for 48 hours. The mixture was filtered and the filtrate was acidified with HCl 37%. The mixture was stirred at room temperature for 30 minutes. The solid was filtered, washed with water and dried in vacuo to provide 225 mg (89 %) of the title compound as a brown solid. MS(m/e): 264.9 (M+H+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Iodo-4-(trifluoromethyl)benzoic acid, its application will become more common.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; KOLCZEWSKI, Sabine; PINARD, Emmanuel; WO2011/23667; (2011); 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. 689260-53-5, name is 2-Bromo-5-iodo-1,3-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C8H8BrI

Under an argon atmosphere, Intermediate 6 (1.20 g, 2.40 mmol), 2-Bromo-5-iodo-1,3-dimethylbenzene (Intermediate 15) (893 mg, 2.88 mmol)(1.68 g, 4.80 mmol, manufactured by Wako Pure Chemical Industries, Ltd.) and copper iodide (91.4 mg, 0.48 mmol, 0.35 mmol) were added to a solution of L-proline (110 mg, 0.96 mmol; manufactured by Wako Pure Chemical Industries, (Manufactured by Wako Pure Chemical Industries, Ltd.) Dimethylformamide (2.4 ml, manufactured by Wako Pure Chemical Industries, Ltd.) was heated to 110 C under an argon atmosphere for 48 hours. to the next,After cooling to room temperature, saturated aqueous ammonium chloride solution (30 ml) and dichloromethane (100 ml) were added to the reaction mixture and the layers were separated. The organic layer was dried over magnesium sulfate and the residue was purified by silica gel column chromatography (dichloromethane 20% Hexane 80%) to obtain Intermediate 16 as pale yellow crystals (1.49 g, yield 91%).

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 689260-53-5.

Reference:
Patent; Kokuritsu Daigaku Hojin Kyushu Daigaku; Kaji, Hironori; Suzuki, Hajime; Suzuki, Katsuaki; Oheiwa, Hajime; Wakamiya, Atsushi; Fukushima, Tatsuya; Suzuki, Huritz; Murata, Yaseujiro; Sieje, Kacheuyuki; Adachi, Jihaya; (48 pag.)KR2015/123907; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 51839-15-7, 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. 51839-15-7 name is Dimethyl 5-iodoisophthalate, 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: A 15 mL heavy walled pressure tube sealable with a gasketed Teflon screwcap was charged with a diaryl iodonium triflate (0.2 mmol, 1 equiv), an aryl iodide (1.0 mmol, 5 equiv.), and 1,2-dicholoroethane (2 mL, 0.1 M iodonium triflate concentration). The tube was sealed (Teflon screw cap) and immersed in an oil bath maintained at 80 C. After the indicated time, the tube was retrieved and cooled to rt and the contents were concentrated under reduced pressure. The crude material was purified by silica gel flash chromatography (gradient 10 ? 50% acetone/CH2Cl2).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Dimethyl 5-iodoisophthalate, and friends who are interested can also refer to it.

Reference:
Article; Racicot, Leanne; Ciufolini, Marco A.; Tetrahedron; vol. 73; 50; (2017); p. 7067 – 7072;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 21740-00-1, 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 21740-00-1 as follows.

General procedure: A mixture of 2-iodobenzoic 1a (0.2 mmol), acetylacetone 2a (0.4 mmol), and Cs2CO3 (65.2 mg, 0.20 mmol) in CH3CN was stirred at 100 C. When the reaction was considered complete as determined by TLC analysis, the reaction was allowed to cool to room temperature and quenched by water, and the mixture was extracted with CH2Cl2. The combined organic extracts were washed with water and saturated brine. The organic layers were dried over Na2SO4, filtered. Solvents were evaporated under reduced pressure. The residue was purified by chromatography on silica gel to afford isocoumarins derivatives and isoquinolone derivatives.

According to the analysis of related databases, 21740-00-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Lei; Hu, Jie; Wang, Xiang-Chuan; Zhong, Mei-Jin; Liu, Xue-Yuan; Yang, Shang-Dong; Liang, Yong-Min; Tetrahedron; vol. 68; 27-28; (2012); p. 5391 – 5395;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com