Category: iodides-buliding-blocks

31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, 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. Safety of 2-Bromo-1-(4-iodophenyl)ethanone

[00212] (Based on J. Med. Chem. 2001, 44, 2990-3000) To a solution of Cbz-D-Ala-OH(5.0 g, 22.4 mmol) in NMP (100 mL) was added cesium carbonate (3.72 g, 11.4 mmol). After stirring at RT for 1 h, 12.2 (7.60 g, 22.4 mmol) was added. The reaction mixture was stirred at room temperature and monitored by LC/MS. The reaction solution was diluted with xylene (100 mL) and ammonium acetate (9.25 g, 120 mmol) and then stirred at 1200C for 4 hours. Up to 50 eq of additional ammonium acetate may be needed depending on the reaction progress. The key is to see solid in the flask at all times. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate (200 mL). The EtOAc solution was washed with saturated sodium bicarbonate solution (200 mL) twice, dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was dissolved in DCM (100 mL) and stirred for 1 h to give a precipitate. Solid 12 (4.Og) was filtered off and dried under vacuum. The mother solution was concentrated by rotovap and the residue purified by preparative HPLC over silica gel to give additional 12 (Hex:EtOAc 1:1 to EtOAc 100%). The two products were combined and dried under vacuum to give a total of 5.8 g of 12 (58%).

The synthetic route of 31827-94-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CYTOKINETICS, INC.; WO2007/56056; (2007); A2;,
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Reference of 98-61-3, A common heterocyclic compound, 98-61-3, name is 4-Iodobenzenesulfonyl chloride, molecular formula is C6H4ClIO2S, 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: In a typical experiment, the alkene derivative (1.5 mmol), halobenzenesulfonyl chloride derivative (1 mmol), Li2CO3 (0.222 g, 3 mmol), and PdCl2(CH3CN)2 (12.9 mg, 0.05 mmol) were dissolved in 1,4-dioxane (2 mL) under an argon atmosphere. The reaction mixture was stirred at 100 C for 24 h. After evaporation of the solvent, the product was purified by silica gel column chromatography.

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:
Article; Skhiri, Aymen; Salem, Ridha Ben; Soule, Jean-Francois; Doucet, Henri; Synthesis; vol. 48; 18; (2016); p. 3097 – 3106;,
Iodide – Wikipedia,
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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 19230-28-5 as follows. Computed Properties of C6H3Cl2I

To a solution of 8-allyl-2- (methylthio) -5-oxo-5, 8- dihydropyrido[2,3-d]pyrimidine-6-carboxylic acid (50 mg,0.18 mmol) in toluene (2 mL) and DMA (0.22 mL) was added1,3-dichloro-2-iodobenzene (98 mg, 0.36 mmol) and silver carbonate (49.7 mg, 0.18 mmol) . The suspension was degassed for 5 mm and (oxybis(2,1- phenylene))bis(diphenylphosphine) (9.7 mg, 0.018 mmol)and palladium (II) chloride (1.6 mg, 9.0 imol) added. The reaction mixture was then heated in a microwave (Biotage Initiator) at 150 C for 1 h. The reaction mixture was concentrated in vacuo and purified by flash chromatography (0-100%, EtOAc in cyclohexane) to affordthe title compound (12.4 mg, 18%) as a yellow solid. LCMS (Method A) : = 1.55 mi m/z = 378 [M+H].

According to the analysis of related databases, 19230-28-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ALMAC DISCOVERY LIMITED; ROUNTREE, James Samuel Shane; O’DOWD, Colin Roderick; BURKAMP, Frank; BELL, Mark Peter; WO2015/19037; (2015); A1;,
Iodide – Wikipedia,
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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,
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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,
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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,
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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

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

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

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