Month: September 2021

Related Products of 214279-40-0, A common heterocyclic compound, 214279-40-0, name is 2-Iodo-4-methoxy-1-nitrobenzene, molecular formula is C7H6INO3, 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.

The title compound was prepared with the analogous procedure described in example 1 using 2-lodo-4-methoxy-1 -nitrobenzene (140 mg, 0.5 mmol) and lambda/-Phenyl- formamide (73 mg, 0.6 mmol) as starting materials to yield the title compound as viscous oil (62 mg, 56%). 1H NMR (DMSO) delta 2.58 (s, 3 H), 2.64 (s, 3 H), 7.37 (d, J = 8.1 Hz, 1 H), 7.44 (dd, J = 8.1 , 7.3 Hz, 1 H), 7.48-7.52 (m, 1 H), 7.54 (d, J = 8.8 Hz, 2 H), 7.61 (d, J = 8.8 Hz, 2 H), 7.86 (d, J = 7.3 Hz, 1 H).

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; SANOFI-AVENTIS; WO2009/413; (2008); 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. 629-09-4, name is 1,6-Diiodohexane, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 629-09-4

To a solution of potassium 1,3-dioxoisoindolin-2-ide (5.0 g, 26.99 mmol) in DMF (50 mL) was added 1,6-Diiodohexane (22.8 g, 67.49 mmol) and the mixture was heated at 70 C for 2.5 h. The reaction was monitored by TLC. After completion, the mixture was diluted with H2O (100 mL) and extracted with EtOAc (200 mL × 2). The combined organic layers were washed with brine (100 mL), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to obtain a crude which was purified by CombiFlash chromatography to afford the title compound. LC-MS 358 [M+H]+

According to the analysis of related databases, 629-09-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NUVATION BIO INC.; PHAM, Son Minh; CHAKRAVARTY, Sarvajit; CHEN, Jiyun; KANKANALA, Jayakanth; BARDE, Anup; NAYAK, Anjan Kumar; HUNG, David; (283 pag.)WO2019/222272; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 401-81-0, 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. 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Catalyst 2c (prepared according Ref. 26b, 133 mg, 6.2 equiv of Pd) was added to a solution of aryl iodide (0.20 mmol, 1.0 m equiv), alkene (0.40 mmol, 2.0 equiv) in DMF (2 mL). The reaction mixture was heated at 100 C for 20 h. After cooling to rt, compound 2c was filtered off under vacuum using a 0.2 mum membrane. The mixture of solvents was concentrated under vacuum to afford pure 3a-j after drying under vacuum (0.1 mbar). The catalyst 2c was then regenerated by reaction with NBu3 (0.16 mL, 0.66 mmol, 3.3 equiv) in DMF at rt for 3 h. Compound 2c was then filtered under vacuum, washed with Et2O (2 mL), and dried under vacuum.

The synthetic route of 1-Iodo-3-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Derible, Antoine; Yang, Yun-Chin; Toy, Patrick H.; Becht, Jean-Michel; Le Drian, Claude; Tetrahedron Letters; vol. 55; 31; (2014); p. 4331 – 4333;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 101335-11-9, A common heterocyclic compound, 101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, molecular formula is C6H3ClFI, 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.

General procedure: To 259 mg (26.9 mmol) pyrimidin-5-ol (J. Chem. Soc. 1956, 2033) in 200 mL DMF are added 108 mg (26.9 mmol) sodium hydride (60% dispersion in mineral oil). The mixture is stirred for 20 mm at r.t.. After that time, 500 mg (22.4 mmol) 2-fluoro-4-iodopyridine are added and the mixture is stirred for 12 h at 80 C. Subsequently the mixture is poured into water and extracted with ethyl acetate (3x). The combined organic layers are washed with brine. After drying over sodium sulphate, the solvent is removed in vacuo and the residue is purified by column chromatography (silica gel; heptane/EtOAc, 100/0 – 40/60).C9H6IN3O (M = 299.1 g/mol)ESI-MS: 300 [M+H]+ Rt(HPLC) : 2.87 min (method C) For the example XXVIII.4 6 eq. of the alcohol and 4 eq. of KOtBu as base are used and the reaction mixture is stirred at r.t. for 3 h.

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; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; FLECK, Martin; ROTH, Gerald Juergen; NOSSE, Bernd; HEINE, Niklas; WO2013/92616; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 19094-56-5, name is 2-Chloro-5-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 19094-56-5, 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 1% 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 <0.06% w/w is obtained. The second half of the organic phase is processed identically. A total of 410 kg (94% yield) of product which has a white to off-white crystalline appearance, is obtained. The identity of the product is determined via infrared spectrometry. 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:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2011/237526; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 444-29-1, A common heterocyclic compound, 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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.

General procedure: A mixture of aryl halides (0.5 mmol), aryl sulfinates (0.75 mmol), Pd(dppf)Cl2 (2.5 mol percent), P(OPh)3 (5 mol percent), K2CO3 (1.5 mmol) and 2 mL of DMF in a schlenk tube was heated to 150 °C under inert atmosphere (24 h for aryl iodides and 26 h for aryl bromides). The reaction mixture was cooled to room temperature, diluted with ethyl acetate and filtered through a plug of Celite. The filtrate was washed sequentially with H2O and brine. The organic layer was separated, dried (Na2SO4), and concentrated under vacuum. The crude product was purified by column chromatography (silica gel; petroleum ether). All the products were analyzed by GC-MS. 1H NMR, 13C NMR and IR of only representative products are given, as all the products are highly reported.

The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gund, Sitaram Haribhau; Balsane, Kishor Eknath; Nagarkar, Jayashree Milind; Tetrahedron; vol. 72; 33; (2016); p. 5051 – 5056;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 640280-28-0, These common heterocyclic compound, 640280-28-0, name is 1-Bromo-2-iodo-4-(trifluoromethyl)benzene, 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 solution of l-bromo-2-iodo-4-(trifluoromethyl)benzene (1.598 ml, 9.70 mmol), tert-butyl 4-(4,4,5,5-tetramethyl-l ,3,2-dioxaborolan-2-yl)-5,6-dihydropyridine-l(2H)- carboxylate (3.00 g, 9.70 mmol), Pd(dppf)-CH2C12 adduct (0.396 g, 0.485 mmol), and potassium carbonate (2.329 g, 38.8 mmol) in 1,4-dioxane (36.4 ml) and water (12.13 ml) was stirred at 70 C for 18 hours. The reaction was diluted with ethyl acetate and washed with water. The aqueous layer was extracted with ethyl acetate, and the combined organic layers were dried with sodium sulfate, filtered, and concentrated. The material was purified via column chromatography (Redi-Sep Gold 80g silica gel column (Teledyne Isco, Lincoln, NE), gradient elution 0 to 100% Et20:Heptane) to afford tert- butyl 4-(2-bromo-5-(trifluoromethyl)phenyl)-5,6-dihydropyridine-l(2H)-carboxylate as a light yellow oil. m/z (ESI) 428.1 (M+Na)+.

The synthetic route of 640280-28-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DINEEN, Thomas; MARX, Isaac, E.; NGUYEN, Hanh, Nho; WEISS, Matthew; AMGEN INC.; WO2013/25883; (2013); 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. 25245-27-6, name is 1-Iodo-3,5-dimethoxybenzene, A new synthetic method of this compound is introduced below., name: 1-Iodo-3,5-dimethoxybenzene

1. Condensation reaction: in with a thermometer, condenser 250 ml four bottle is added between the 26.7g 5 – iodo – teredimethyl ether, 12.8g bromopropylene, 20.4g triethylamine, 2.2g dppp nickel chloride, 130 ml methyl tert-butyl ether, magnetic stirring, oil bath heating, when the temperature rises to 80 C and maintaining at 4 hours, after the reaction is cooled to ambient temperature, for 60 ml 10% hydrochloric acid aqueous solution washing the reaction liquid, water washed to neutral, the organic layer is distilled under reduced pressure to obtain between the 21.4g 5 – propenyl – teredimethyl ether, yield 96.1%.

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; Weifang Xian Da Chemical Co., Ltd.; Li Kai; Wang Guangyue; Yang Qiwei; Zou Yabo; (7 pag.)CN106748673; (2017); 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, category: iodides-buliding-blocks

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

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 34270-90-1 as follows. Computed Properties of C4H8I2O

A mixture of compound 1 (1 mmol), 1-iodo-2-(2-iodoethoxy)ethane (1 mmol) and anhydrouspotassium carbonate (140 mg, 1 mmol) in anhydrous acetonitrile (10 mL) was heated under reflux for1 h and then quenched with water (5 mL). Product 47 was extracted with ethyl acetate and purified ona chromatotron eluting with dichloromethane/methanol (8:2).Yield 66%; m.p. >200 C (decomp.); 1H-NMR (DMSO-d6): delta 8.55 (m, 1H), 8.46 (d, J = 5.2 Hz, 1H), 7.83(m, 1H), 7.10 (m, 2H), 4.13 (m, 4H), 3.98 (m, 4H), 3.74 (m, 4H), 3.67 (m, 4H). HR-MS (ESI). Calcd forC16H21N4O2 (M+): m/z 301.1665. Found: m/z 301.1650. Anal. Calcd for C16H21N4IO2: C, 44.87; H, 4.94;N, 13.08. Found: C, 44.97; H, 5.09; N, 12.69.

According to the analysis of related databases, 34270-90-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Strekowski, Lucjan; Saczewski, Jaros?aw; Raux, Elizabeth A.; Fernando, Nilmi T.; Klenc, Jeff; Paranjpe, Shirish; Raszkiewicz, Aldona; Blake, Ava L.; Ehalt, Adam J.; Barnes, Samuel; Baranowski, Timothy C.; Sullivan, Shannon M.; Sata?a, Grzegorz; Bojarski, Andrzej J.; Molecules; vol. 21; 4; (2016);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com