Month: June 2021

Reference of 216393-67-8, 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 216393-67-8 as follows.

4~Chloro-2-fluoro-6-iodoaniline (Intermediate 30, 1.35 g, 5 mmol), pyruvic acid (1.32 g,15 mmol) and DABCO (1.68 g,15 mmol) were dissolved in DMF(15 mL). The solution was degassed and palladium acetate (56 mg) was added. The mixture was then heated to 1000C for 3h., cooled to ambient and filtered. The filtrate was diluted with EtOAc (100 mL), washed with 2M HCl (2 x 2OmL), water (20 mL) and brine (20 mL), dried (MgSO4) and evaporated to leave the title compound as a dark solid (0.9g, 85% ). 1H NMR (400 MHz, DMSO-de) delta 7.16 (IH, t), 7.21 – 7.24 (IH, m), 7.59 (IH, d), 12.52 (IH, s), 13.27 (IH, s); MS m/z 212 (M-H)”

According to the analysis of related databases, 216393-67-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/82400; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 98-61-3, 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. 98-61-3, name is 4-Iodobenzenesulfonyl chloride belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 4-iodobenzenesulfonyl chloride 1 (500 mg, 1 66 mmol) in anhydrous acetomtrile (8 mL) under a nitrogen atmosphere was added pyrrolidine 2 (140 mg, 1 97 mmol) and pyridine (261 mg, 3 3 mmol) The reaction mixture was stirred at room temperature for 3 hours Ethyl acetate (100 mL) was added and the organic layer was washed with 1 N hydrochloric acid, water and brine The organic layer was dried over anhydrous sodium sulfate The organic solvent was evaporated under reduced pressure The crude product was purified by flash column chromatography to afford the desired l-[(4-iodobenzene)sulfonyl]pyrrohdme compound 78-1 (487 mg, 1 45 mmol)

The synthetic route of 4-Iodobenzenesulfonyl chloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MOCHIDA PHARMACEUTICAL CO., LTD.; SCHERING CORPORATION; NISHIDA, Hidemitsu; SAITOH, Fumihiko; HIRABAYASHI, Tomokazu; CHACKALAMANNIL, Samuel; CHAN, Tin-Yau; CHELLIAH, Mariappan, V.; CLASBY, Martin, C.; DWYER, Michael, P.; GREENLEE, William, J.; XIA, Yan; WO2010/65717; (2010); 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., COA of Formula: C4H8ClI

(Step 2) [1-(2-Hydroxyethyl)imidazolidin-2-ylidene] malononitrile (2.00 g, 11.2 mmol) obtained in the Step 1 was dissolved in DMF (20 mL) and the solution was sequentially added with potassium carbonate (3.10 g, 22.4 mmol) and 1-chloro-4-iodobutane (2.75 mL, 22.4 mmol). After stirring the mixture at room temperature for 71 hours, potassium carbonate (3.10 g, 22.4 mmol) and 1-chloro-4-iodobutane (2.75 mL, 22.4 mmol) were added, followed by stirring at 35°C for 6 hours and at a room temperature for 14 hours. The mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The residue was washed with diisopropylether to obtain [1-(4-chlorobutyl)-3-(2-hydroxyethyl)imidazolidin-2-ylidene]malononitrile (2.55 g, 84.6percent) as a white solid. 1H NMR (CDCl3, deltappm): 1.87-1.99 (m, 2H), 2.12-2.24 (m, 2H), 3.61-3.76 (m, 12H).

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; KYOWA HAKKO KOGYO CO., LTD.; EP1847530; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 19099-54-8, A common heterocyclic compound, 19099-54-8, name is 1-Iodo-2-isopropylbenzene, molecular formula is C9H11I, 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.

0.3 mmol of sodium carbonate, N-(3-(4-methoxyphenyl)prop-2-yn-1-yl)-4-methylbenzenesulfonamide0.1mmol,Tetrakis(triphenylphosphine palladium) 0.005 mmol, bis(2-diphenylphosphinophenyl)ether 0.005 mmol,0.2 mmol of 4-methylbenzeneboronic acid, 0.3 mmol of 2-isopropyliodobenzene, and 1 mL of N,N-dimethylformamide were added to a 15 mL reaction tube.Nitrogen was repeatedly filled 10 times, placed in an oil bath at 120 C, and reacted for 24 hours;Cooled to room temperature, the reaction was diluted with ethyl acetate, washed with water three times, the organic phase dried over anhydrous Na2SO4, filtered, and concentratedPurification by thin layer chromatography to give 21.5mg of the desired product, yield 41%.

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; Huaqiao University; Cheng Guolin; Lv Weiwei; (20 pag.)CN109879713; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. Recommanded Product: 640280-28-0

A vial was charged with N-(2,4-dimethoxybenzyl)-l-methyl-3-(4,4,5,5- tetramethyl-l,3,2-dioxaborolan-2-yl)-N-(l,2,4-thiadiazol-5-yl)-lH-indole-6-sulfonamide (.500 g, 0.876 mmol), 2-bromo-l-iodo-4-(trifluoromethyl)benzene (0.769 g, 2.191 mmol), potassium phosphate (0.651 g, 3.07 mmol), and PdCi2(dppf)-CH2Ci2 (0.072 g, 0.088 mmol). DMF (5.84 ml), and the vial was flushed with argon, sealed, and stirred at 60 C for two 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 washed with brine, dried with sodium sulfate, filtered, and concentrated. The material was purified via column chromatography (silica gel, gradient elution 0 to 100% EtOAc:Hexanes) to afford 3-(2-bromo-4-(trifluoromethyl)phenyl)-N-(2,4- dimethoxybenzyl)-l-methyl-N-(l ,2,4-thiadiazol-5-yl)-lH-indole-6-sulfonamide (.255 g, 0.382 mmol, 43.6 % yield) as an off-white solid, m/z (ESI) 667.0 (M+H)+.

The synthetic route of 1-Bromo-2-iodo-4-(trifluoromethyl)benzene 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

Adding a certain compound to certain chemical reactions, such as: 620-05-3, name is (Iodomethyl)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 620-05-3, COA of Formula: C7H7I

General procedure: A mixture of 4-oxo-1,4-dihydroquinoline-2-carboxylic acid alkylester (1, 1 mmol), base (1.3 mmol), the corresponding alkylatingagent (alkyl iodide, 1.5 mmol; others, 1.2 mmol) and anhydrousDMF (5 mL) was stirred at the appropriate temperature andmonitored by TLC (DCM:MeOH 4.7:0.3). After a specified time(Table 2), the mixture was carefully poured into ice-water. Thecompounds obtained were isolated and purified as was indicatedabove. Alkylating agents, bases and solvents are presented inTable 2.

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, (Iodomethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Shmidt, Maria S.; Arroyo Manez, Pau; Stortz, Carlos A.; Perillo, Isabel A.; Vega, Daniel; Blanco, Maria M.; Journal of Molecular Structure; vol. 1128; (2017); p. 142 – 150;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 112671-42-8, 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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows.

(1) Add dibenzothiophene-1-boronic acid (100mmol), 2-iodo-5-bromonitrobenzene (100mmol), 0.9g (0.785mmol, 0.5%) tetratriphenylphosphine palladium, 500mL of toluene, 200mL of ethanol, 200mL of water and 40g (300mmol) of potassium carbonate, react at 100 C for 8h; after the reaction is complete, stop the reaction; cool to room temperature, separate the organic phase, concentrate, silica gel column chromatography to obtain yellow powder M1;

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

Reference:
Patent; Yantai Xianhua Chemical Technology Co., Ltd.; Xing Qifeng; Feng Peichuan; Chen Yue; Hu Lingfeng; Chen Yili; (24 pag.)CN110734446; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 335349-57-0,Some common heterocyclic compound, 335349-57-0, name is 5-Chloro-4-iodo-2-nitroaniline, molecular formula is C6H4ClIN2O2, 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 B1 (5-Chloro-4-iodo-2-nitro-phenyl)-carbamic acid tert.-butyl ester The title compound was prepared via the isocyanate from 5-chloro-4-iodo-2-nitro-phenylamine (Example A1) (7.0 g, 23.45 mmol) with diphosgene (2.12 mL, 17.6 mmol) in EtOAc (30 mL), followed by treatment with tert.-BuOH (100 mL) in CH2Cl2 (100 mL) according to the general procedure B (method a). Obtained as a yellow solid (7.1 g, 76%). MS (EI) 398 (M+) and 400 [(M+2)+]; mp 82-84 C.

The synthetic route of 335349-57-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffman-La Roche Inc.; US6544985; (2003); B2;,
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. 34883-46-0, name is 1-Iodo-2-phenoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 34883-46-0

General procedure: Intermediate Bn (1.0 eq) was dissolved in 120 mL of anhydrous tetrahydrofuran (THF) (0.4M), and cooled to -78 C. n-Butyllithium (n-BuLi)(2.5 M, 1.0 eq) was slowly added to the above cooled solution, and the reaction mass was stirred for 1 h. After 1 h of stirring, Intermediate An (0.7 eq) was added to the reaction solution and stirred for additional 3 h at 25 C. After the completion of the reaction, it was quenched by saturated solution of ammonium chloride, and extracted with organic solvent. The organic layer was separated, concentrated, and recrystallized with petroleum ether to obtain a white solid product.

The synthetic route of 34883-46-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NICHEM FINE TECHNOLOGY CO., LTD.; LU, Tai-Ni; WU, Hui-Ling; SHIEH, Shwu-Ju; CHEN, Chi-Chung; (108 pag.)US2019/92745; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 40400-15-5,Some common heterocyclic compound, 40400-15-5, name is 2-(2-Iodophenyl)acetonitrile, molecular formula is C8H6IN, 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.

Under a protective atmosphere of inert gas, Pd(OAc)2 (2.2 mg, 10 mol%), XPhos (19.1 mg, 20 mol%), NBE-CO2K (3.5 mg, were added to a 4.0 mL reaction flask equipped with a magnetic stir bar. 10 mol%), 2-(2-iodophenyl)acetonitrile (0.2 mmol, 1.0 equiv.), ethylene oxide (0.6 mmol, 3.0 equiv.) and dry N-methylpyrrolidone(1.0 mL). The reaction flask was capped and stirred at room temperature for about 5 minutes, after which the mixture was heated to 80 C and stirred for 24 hours.After the reaction vessel was cooled to room temperature, it was quenched with water (10 mL), extracted with methyl tert-butyl ether (3×10 mL), dried over Na2SO4Filter and concentrate under vacuum. Purified by column chromatography, the eluent was petroleum ether: ethyl acetate = 20:1 (v/v).There was obtained 26 mg of 2-(2,3-dihydrobenzofuran-7-yl)acetonitrile (colorless oily liquid, yield 82%).

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

Reference:
Patent; Wuhan University; Zhou Qianghui; Wu Chenggui; Cheng Honggang; (20 pag.)CN108329285; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com