Category: 19094-56-5

Electric Literature of 19094-56-5, The chemical industry reduces the impact on the environment during synthesis 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, I believe this compound will play a more active role in future production and life.

General procedure: To a stirred suspension of 2-chloro-5-iodobenzoic acid(5.65 g, 0.02 mol) in CH2Cl2(20 mL) was added oxalylchloride(1.80 mL, 0.021 mol) and DMF(0.02 mL). Theresulting mixture was stirred for 4 h at room temperature.The mixture was concentrated, and the residual colorlesssolid was dissolved in CH2Cl2(40 mL). To this solutionwere added corresponding substituted benzene(0.02 mol)and then AlCl3(2.75 g, 0.021 mol) portionwise so that thetemperature did not exceed 0 C. After being stirred at 10-20 C for 3 h, the mixture was poured into ice water andextracted with CH2Cl2 three times. The combined organiclayers were washed with 1M HCl, water, and brine, thendried over MgSO4 and concentrated. The residual solid wascrystallized from ethanol to give as white solid.According to this procedure the following compoundswere prepared.

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, 2-Chloro-5-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Hu, Shengquan; Sun, Wuji; Wang, Yeming; Yan, Hong; Medicinal Chemistry Research; vol. 28; 4; (2019); p. 465 – 472;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 19094-56-5, 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. 19094-56-5, name is 2-Chloro-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2-Chloro-5-iodobenzoic acid (10.0 g, 35.3 mmol) And suspended in methylene chloride (200 mL). N, N-Dimethylformamide (0.05 mL) was added to the resulting mixture, followed by the dropwise addition of oxalyl chloride (11.3 g, 89.0 mmol) at 0 C. After completion of the dropwise addition, the resulting mixture was allowed to warm to room temperature and stirred for 4 hours. The resulting clear solution was evaporated by rotary evaporation to remove the solvent and yielded 10.7 g of product in 100% yield, which was used directly in the next reaction without purification.

The synthetic route of 2-Chloro-5-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SENJU Pharma Corporation Limited; Woo, Frank; (28 pag.)KR2015/81220; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 19094-56-5, These common heterocyclic compound, 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, 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.

Example 1 : Synthesis of the fluoride VIII.1Oxalylchloride (176kg; 1386mol; 1 ,14eq) is added to a mixture of 2-chloro-5-iodo benzoic acid (343kg; 1214mol) (compound IX.1 ), fluorobenzene (858kg) and N,N- dimethylformamide (2kg) within 3 hours at a temperature in the range from about 25 to 30°C (gas formation). After completion of the addition, the reaction mixture is stirred for additional 2 hours at a temperature of about 25 to 30°C. The solvent (291 kg) is distilled off at a temperature between 40 and 45°C (p=200mbar). Then the reaction solution (91 1 kg) is added to aluminiumchloride AICI3 (181 kg) andfluorobenzene (192kg) at a temperature between about 25 and 30°C within 2 hours. The reaction solution is stirred at the same temperature for about an additional hour. Then the reaction mixture is added to an amount of 570 kg of water within about 2 hours at a temperature between about 20 and 30°C and stirred for an additional hour. After phase separation the organic phase (1200kg) is separated into two halves (600kg each). From the first half of the organic phase solvent (172kg) is distilled off at a temperature of about 40 to 50°C (p=200mbar). Then 2-propanole (640kg) is added. The solution is heated to about 50°C and then filtered through a charcoal cartouche (clear filtration). The cartouche may be exchanged during filtration and washed with a fluorobenzene/2-propanole mixture (1 :4; 40kg) after filtration. Solvent (721 kg) is distilled off at a temperature of about 40 to 50°C and p=200mbar. Then 2-propanole (240kg) is added at a temperature in the range between about 40 to 50°C. If the content of fluorobenzene is greater than 1 percent as determined via GC, another 140kg of solvent are distilled off and 2-propanole (140kg) is added. Then the solution is cooled from about 50°C to 40°C within one hour and seeding crystals (50g) are added. The solution is further cooled from about 40°C to 20°C within 2 hours. Water (450kg) is added at about 20°C within 1 hour and the suspension is stirred at about 20°C for an additional hour before the suspension is filtered. The filter cake is washed with 2-propanole/water (1 :1 ; 800kg). The product is dried until a water level of <0.06percentw/w is obtained. The second half of the organic phase is processed identically. A total of 410kg (94percentyield) of product which has a white to off-white crystalline appearance, is obtained. The identity of the product is determined via infrared spectrometry. The synthetic route of 19094-56-5 has been constantly updated, and we look forward to future research findings. Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; WEBER, Dirk; RENNER, Svenja; FIEDLER, Tobias; ORLICH, Simone; WO2011/39107; (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. 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 2-Chloro-5-iodobenzoic acid

A solution of 2-chloro-5-iodobenzoic acid (28 g, 99 mmoles) and toluene (198 ml.) was cooled to O0C. A 1 M diisobutyl aluminium hydride (DIBAL) solution in toluene 208 ml_, 208 mmol) solution was added drop wise over 20 minutes. The solution was allowed to slowly warm to rt. After 16 h the solution was cooled to O0C, MeOH and 1 M HCI was slowly added (exothermic reaction). The solution became clumpy and was filtered and the clumps washed with EtOAc. The organic phase was then isolated and the aqueous layer washed with EtOAc. The combined organic extracts were then washed with brine, dried (Na2SO4), and concentrated. The product was purified by Biotage chromatography (0% – 100% EtOAc/Hexanes) to afford 9.01 g of product as a solid (34%). 1H NMR (400 MHz, chloroform- cQ delta ppm 7.85 (d, J=2.02 Hz, 1 H) 7.55 (dd, J=8.34, 2.27 Hz, 1 H) 7.09 (d, J=8.34 Hz, 1 H) 4.74 (s, 2 H) 2.25 (s, 1 H).

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 19094-56-5.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2008/77009; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

19094-56-5, name is 2-Chloro-5-iodobenzoic acid, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. name: 2-Chloro-5-iodobenzoic acid

Example 3; 4′-Chloro-3′-[[(cyclohexylmethyl)amino]carbonyl]-[l,l’-biphenyl]-2-carboxylic acid; EPO a) 2-Chloro-5-iodo-benzoic acid, 1,1-dimethylethyl ester; iV,iV-Dimethylformamide (1 drop) and oxalyl chloride (4.8 mL) were added to a stirred solution of 2-chloro-5-iodobenzoic acid (5 g) in dichloromethane (20 mL) at 0 C. The reaction was allowed to warm to room temperature, stirred under nitrogen for 2 hours, and then evaporated to dryness. The residue was dissolved in tetrahydrofuran (20 mL) and cooled to 0 0C. Potassium terf-butoxide (22 mL, 1 M solution in tetrahydrofuran) was added over 10 minutes. The reaction was allowed to warm to room temperature and stirred under nitrogen for 2 hours then poured into saturated aqueous sodium bicarbonate (50 mL). The layers were separated and the aqueous was extracted with diethyl ether (50 mL). The combined organics were dried, filtered and evaporated to afford the sub-title compound as an oil (5.7 g).1HNMR (400 MHz, d6-DMSO) delta 7.99 (IH, d), 7.87 (IH5 dd), 7.34 (IH, d), 1.54 (9H, s).

The synthetic route of 19094-56-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; WO2006/80884; (2006); 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. 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, A new synthetic method of this compound is introduced below., Formula: C7H4ClIO2

[0256] A I L 4-necked flask equipped with thermometer and mechanical stirrer (operating at 150 RPM) was charged with 2-chloro-5-iodobenzoic acid (14.1 g, 0.05 mol), DCM (70.5 mL) and oxalyl chloride (5.5 mL, 0.06 mol). After stirring for 10 min, the mixture was cooled to 10 to 15 C and DMF (0.15 mL, 1.92 mmol) was added by syringe over 10 min in two boluses of 0.1 and 0.05 mL while keeping the reaction temperature below 20 C. After the addition was completed, the mixture was warmed to 25 C and stirred for 16 h. The mixture was concentrated and the residue was dried under vacuum at 30 C for 5 h to give 15.0 g of product as a white solid. Yield: 100%. LC-MS Method EGT-M-0013: 99 % Purity, 1H NMR (CDCI3, 400 MHz): 8.33 (d, J=2.4 Hz, 1H), 7.81-7.84 (dd, J=2.4 Hz, 8.4 Hz, 1H), 7.23 (d, J=8.4 Hz, 1H).

The synthetic route of 19094-56-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THERACOS, INC.; XU, Baihua; LV, Binhua; XU, Ge; SEED, Brian; ROBERGE, Jacques; WO2013/152476; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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 19094-56-5 as follows. Safety of 2-Chloro-5-iodobenzoic acid

5-iodoaniline-2-chlorobnenzoic acid 3. 3g soln. ethanol 150 ml, concentrated hydrochloric acid 0. 11g is added, heated under reflux for 12 hours. After returning the reaction solution to room temperature, is diluted with water, adding an aqueous solution of sodium hydroxide 1N, 3 times extracted with ethyl acetate. The organic layer, washed with saturated saline solution, dried with magnesium sulfate waterlessly org. layer. By concentrating the pressure somas, 5-iodoaniline-2-ethyl chlorobnenzoic (43) 1. 74g is obtained.

According to the analysis of related databases, 19094-56-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; OAT AGRIO COMPANY LIMITED; UENAKA, GO; MASUMOTO, SATORU; HAYASHI, NAOTAKA; (63 pag.)JP5743418; (2015); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 19094-56-5, 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. 19094-56-5, name is 2-Chloro-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of 2-chloro-5-iodo-benzoic acid (25.63 g, 90 mmol) in methanol (500 ML) saturated with HCL gas was stirred at room temperature for 48H. The reaction mixture was concentrated I71 vacuo, diluted with 1: 1 ethyl ACETATE/DIETHYL ether and washed with saturated aqueous sodium bicarbonate and brine. The organiclayer was dried over sodium sulfate, filtered and concentrated ILL vacuo to afford the title compound (25.0 g).

The synthetic route of 2-Chloro-5-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PFIZER PRODUCTS INC.; WO2004/99146; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

19094-56-5, name is 2-Chloro-5-iodobenzoic acid, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C7H4ClIO2

Oxalylchloride (176 kg; 1386 mol; 1.14 eq) is added to a mixture of 2-chloro-5-iodo benzoic acid (343 kg; 1214 mol) (compound IX.1), fluorobenzene (858 kg) and N,N-dimethylformamide (2 kg) within 3 hours at a temperature in the range from about 25 to 30° C. (gas formation). After completion of the addition, the reaction mixture is stirred for additional 2 hours at a temperature of about 25 to 30° C. The solvent (291 kg) is distilled off at a temperature between 40 and 45° C. (p=200 mbar). Then the reaction solution (911 kg) is added to aluminiumchloride AlCl3 (181 kg) and fluorobenzene (192 kg) at a temperature between about 25 and 30° C. within 2 hours. The reaction solution is stirred at the same temperature for about an additional hour. Then the reaction mixture is added to an amount of 570 kg of water within about 2 hours at a temperature between about 20 and 30° C. and stirred for an additional hour. After phase separation the organic phase (1200 kg) is separated into two halves (600 kg each). From the first half of the organic phase solvent (172 kg) is distilled off at a temperature of about 40 to 50° C. (p=200 mbar). Then 2-propanole (640 kg) is added. The solution is heated to about 50° C. and then filtered through a charcoal cartouche (clear filtration). The cartouche may be exchanged during filtration and washed with a fluorobenzene/2-propanole mixture (1:4; 40 kg) after filtration. Solvent (721 kg) is distilled off at a temperature of about 40 to 50° C. and p=200 mbar. Then 2-propanole (240 kg) is added at a temperature in the range between about 40 to 50° C. If the content of fluorobenzene is greater than 1percent as determined via GC, another 140 kg of solvent are distilled off and 2-propanole (140 kg) is added. Then the solution is cooled from about 50° C. to 40° C. within one hour and seeding crystals (50 g) are added. The solution is further cooled from about 40° C. to 20° C. within 2 hours. Water (450 kg) is added at about 20° C. within 1 hour and the suspension is stirred at about 20° C. for an additional hour before the suspension is filtered. The filter cake is washed with 2-propanole/water (1:1; 800 kg). The product is dried until a water level of <0.06percent w/w is obtained. The second half of the organic phase is processed identically. A total of 410 kg (94percent yield) of product which has a white to off-white crystalline appearance, is obtained. The identity of the product is determined via infrared spectrometry. The synthetic route of 19094-56-5 has been constantly updated, and we look forward to future research findings. Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2011/237789; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 19094-56-5, These common heterocyclic compound, 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, 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 dried flask, 5-iodo-2-chlorobenzoic acid (20.0 g, 70.8 mmol) and dichloromethane (60 mL) were added. The reaction mixture was stirred, then oxalyl chloride (9.8 g, 77.9 mmol) and DMF (0.2 mL) were slowly added dropwise, and some bubbles were observed. The reaction mixture was stirred at room temperature for 7 hours. The solvent and excess oxalyl chloride were removed by rotary evaporation to give a gray solid, which was used directly in the next step without further purification.

The synthetic route of 19094-56-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangsu Hansoh Pharmaceutical Co., Ltd.; ZHONG, Huijuan; LIAO, Jianchun; YU, Hongping; XU, Yaochang; LI, Qing; CHEN, Jianghua; GAO, Peng; TAN, Songliang; WANG, Shaobao; (45 pag.)US2016/222047; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com