Category: iodides-buliding-blocks

Electric Literature of 626-01-7, 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. 626-01-7 name is 3-Iodoaniline, 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: In a test tube equipped with a magnetic stirrer bar, thearyl halide 1 (1 mmol) was mixed with phenyl boricacid 2 (1.2 mmol), K2CO3(2 mmol), and the Pd-catalyst(0.1mol% Pd) in 2 ml of H2Oin air. The reaction mixturewas then stirred at 50 C for appropriate time. After completionof the reaction, the catalyst was removed by magnetand washed with ethanol and water (3 ¡Á 5 ml). The aqueouslayer was extracted with chloroform, then organic layerdried over anhydrous MgSO4.The solvent was evaporatedunder reduced pressure to give the corresponding biarylcompounds. All the products were previously reported [5,8-12] and were confirmed by the spectroscopic methodusing 1H and 13C NMR (see supporting information).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Iodoaniline, and friends who are interested can also refer to it.

Reference:
Article; Sarvi, Iraj; Gholizadeh, Mostafa; Izadyar, Mohammad; Catalysis Letters; vol. 147; 5; (2017); p. 1162 – 1171;,
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. 20555-91-3, name is 1,2-Dichloro-4-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 20555-91-3

A microwave vial was charged with palladium acetate (0.165 g, 0.733 mmol), l,2-dichloro-4-iodobenzene (2.00 g, 7.33 mmol), but-3-en-2-ol (0.793 g, 1 1.0 mmol), tetrabutylammonium chloride, hydrate (2.17 g, 7.33 mmol), and sodium bicarbonate (1.539 g, 18.32 mmol). DMF (5 mL) was added via syringe and the reaction mixture was degassed three times. The mixture was heated at 60 C for 16 h. The reaction mixture was allowed to cool to room temperature, and diluted with ether. The organic layer was washed with water, separated, dried with MgSC^, filtered and concentrated. The crude residue was purified by silica gel chromatography with an eluant of 10% ethyl acetate / hexanes to afford the desired product Intermediate 4A (1.4 g, 6.5 mmol, 88% yield). LC- MS (ESI) m/z 216.9 (M+H), RT = 2.01 min (Method B).

According to the analysis of related databases, 20555-91-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; HU, Carol Hui; QIAO, Jennifer X.; WANG, Tammy C.; WO2013/151923; (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. 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

Under an argon atmosphere, a suspension of lithium chloride (113 mg, 2.66 mmol) in THF (5.3 mL)A THF solution (2 M, 1.33 mL, 2.66 mmol) of isopropyl magnesium chloride and 1-iodo-4- (trifluoromethyloxy) benzene (0.425 mL, 2.76 mmol) were added at room temperature,And the mixture was stirred for 3 hours.A solution of 2-fluoro-N-methyl-N-methyloxy-2- (1,2,4-triazol-1-yl) acetamide (200 mg, 1.06 mmol) in THF (3.5 mL) In addition,And the mixture was stirred at that temperature for 10 minutes.Saturated ammonium chloride aqueous solution was added to the reaction solution,And extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure.The obtained crude product was purified by column chromatography (hexane: ethyl acetate = 10: 1 to 2: 1)2-fluoro-2- (1,2,4-triazol-1-yl) -1- [4- (trifluoromethyloxy) phenyl] ethanoneWhite solids(218 mg, yield: 71percent).

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; SAGAMI CHEMICAL RESEARCH INSTITUTE; HOKKO CHEMICAL INDUSTRY COMPANY LIMITED; HANDA, MASAMI; MIZUTA, SATOSHI; HIRAI, KENJI; OKAMURA, DAIGO; GUSHIKAWA, TORU; (111 pag.)JP2015/848; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 112671-42-8, The chemical industry reduces the impact on the environment during synthesis 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, I believe this compound will play a more active role in future production and life.

Intermediate M1-a (3.7 g, 18.6 mmol) and 2-iodo-5-bromonitrobenzene (15.3 g, 46.7 mmol), sodium tert-butoxide (7.1 g, 74.4 mmol), toluene 100 mL, nitrogen, Pd2 (dba) 3 (0.3g), tri-tert-butylphosphine (20ml, 10% in toluene solution), start stirring, heat to 100 C reflux, reaction 12h, the reaction liquid is washed, the organic phase is concentrated, passed the silica gel column, eluent For petroleum ether: ethyl acetate = 50:1, the eluent was concentrated to give intermediate M1-b (9.2 g, yield 82.7%).

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, 4-Bromo-1-iodo-2-nitrobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Beijing Dingcai Technology Co., Ltd.; Gu’an Dingcai Technology Co., Ltd.; Fan Hongtao; Zhang Yaguang; Zhang Xianghui; Ren Xueyan; (40 pag.)CN108341825; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 25309-64-2, 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. 25309-64-2, name is 1-Ethyl-4-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: An appropriate phenylacetamide (0.12 mmol, 1 equiv), an appropriate iodo compound (0.48 mmol, 4 equiv), Pd(OAc)2 (2.7 mg, 10 mol%), and AgOAc (50 mg, 0.3 mmol, 2.5 equiv) in anhydrous toluene (3 mL) was heated at 110 C for 24 h under a nitrogen atmosphere. After the reaction period, the solvent was evaporated in vacuo to afford a crude reaction mixture. Purification of the crude reaction mixture by column chromatography furnished the corresponding arylated products 4a-q/7a-f (bis arylation products), 3o,r/6a,b/8e,f/9a,b (mono arylation products) (see corresponding Tables/Schemes for specific examples and reaction conditions).

The synthetic route of 1-Ethyl-4-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bisht, Narendra; Babu, Srinivasarao Arulananda; Tetrahedron; vol. 72; 39; (2016); p. 5886 – 5897;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 6293-83-0, name is 2-Iodo-4-nitroaniline, 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. name: 2-Iodo-4-nitroaniline

A. 1-Chloro-2-iodo-4-nitro-benzene (801A) 2-amino-5-nitro-iodobenzene (10.00 g, 37.9 mmol) was suspended in 12 N HCl (25 mL) and water (40 mL) and stirred for 30 min at 22 C. The mixture was then cooled to 0 C. and NaNO2 (5.23 g, 75.8 mmol in 18 mL of H2O) was added over a 10 min period. After 1 h, this solution was transferred to a solution of CuCl (3.75 g, 37.9 mmol) in water (50 mL) at 60 C. After 2 h, the mixture was cooled to 22 C. and extracted with EtOAc (3*150 mL) and the organics were dried over anhydrous MgSO4. The crude product was purified by silica gel flash chomatography eluding with 10-20% CH2Cl2 in hexanes to give compound 801A (4.20 g) as a yellow solid. HPLC: 100% at 3.447 min (retention time) (YMC S5 ODS column 4.6*50 mm eluding with 10-90% aqueous methanol over 4 mincontaining 0.2% phosphoric acid, 4 mL/min, monitoring at 220 nm).

The synthetic route of 2-Iodo-4-nitroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Salvati, Mark E.; Balog, James Aaron; Pickering, Dacia A.; Giese, Soren; Fura, Aberra; Li, Wenying; Patel, Ramesh N.; Hanson, Ronald L.; Mitt, Toomas; Roberge, Jacques Y.; Corte, James R.; Spergel, Steven H.; Rampulla, Richard A.; Misra, Raj N.; Xiao, Hai-Yun; US2004/77605; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 31827-94-8, A common heterocyclic compound, 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, molecular formula is C8H6BrIO, 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: The appropriate carbonyl compound (50 mmol) was dissolved in 50 mL of ethanol and magnetically stirred with an equimolar quantity of thiosemicarbazide for 24 h at room temperature with catalytic amounts of acetic acid. The desired thiosemicarbazone precipitated from reaction mixture, was filtered, crystallized from suitable solvent, and dried. Equimolar quantities of 4-iodo-acetophenone and bromine, both dissolved in chloroform, were stirred for 4 h at room temperature until the presence of HBr disappeared. The solution was evaporated under vacuum and the obtained pale yellow solid was washed with petroleum ether to give alpha-bromo-4-iodo-acetophenone in good yield (94%). Equimolar amounts of the prepared thiosemicarbazone (50 mmol) and alpha-bromo-4-iodo-acetophenone (50 mmol), both suspended in 50 mL of ethanol, were reacted at room temperature under magnetic stirring for 10 h. The precipitate was filtered and purified by chromatography to give compounds 1-25 in high yield.

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

Reference:
Article; Secci, Daniela; Bizzarri, Bruna; Bolasco, Adriana; Carradori, Simone; D’Ascenzio, Melissa; Rivanera, Daniela; Mari, Emanuela; Polletta, Lucia; Zicari, Alessandra; European Journal of Medicinal Chemistry; vol. 53; (2012); p. 246 – 253;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 2142-70-3, 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. 2142-70-3, name is 1-(2-Iodophenyl)ethanone, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A mixture of Cu2O (Sigma-Aldrich, 99.99% purity, 0.147 mmol), Cs2CO3 (2.94 mmol),distilled water (0.2 mL), aryl halide (1.47 mmol) and p-toluenesulfonic acid (TsOH) solution(0.3 mL, 2.45 mol/dm3) were added to a reaction vial and a screw cap was fitted to it. Thereaction mixture was stirred under air in a closed system at 120 C for 24 h, following whichthe heterogeneous mixture was cooled to room temperature and diluted with dichloromethane.The combined organic extracts were dried with anhydrous Na2SO4 and the solvent wasremoved under reduced pressure. The crude product loaded into the column using minimalamounts of dichloromethane and was purified by silica-gel column chromatography to affordthe N-arylated product. The identity and purity of products was confirmed by 1H and 13CNMR spectroscopic analysis.

The chemical industry reduces the impact on the environment during synthesis 1-(2-Iodophenyl)ethanone. I believe this compound will play a more active role in future production and life.

Reference:
Article; Tan, Bryan Yong-Hao; Teo, Yong-Chua; Synlett; vol. 27; 12; (2016); p. 1814 – 1819;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 6293-83-0, name is 2-Iodo-4-nitroaniline, molecular formula is C6H5IN2O2, 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: 6293-83-0

A2 (100 mg, 378.8 mumol), acetylacetone (46.43 muL, 454.5 mumol), cuprous oxide (5.4 mg, 37.9 mumol), and cesium carbonate (123.4 mg, 378.8 mumol) were added to a 10 mL two-neck round bottom flask. A mixed solvent of N,N-dimethylformamide (0.75 mL) and water (0.25 mL) was replaced with nitrogen in the reaction system for 5 minutes, and then reacted at 100 C for 5 hours. After the reaction was detected by TLC, the reaction solution was cooled to room temperature. Ethyl acetate (2 mL) was added to dilute the reaction solution, and the insoluble impurities were filtered. The filtrate was extracted with ethyl acetate (5 mL ¡Á 3). The organic phases were combined and saturated brine (10 mL) was used. After washing, drying over anhydrous sodium sulfate, filtering the desiccant, and concentrating the filtrate to obtain a residue. Silica gel column chromatography (petroleum ether / ethyl acetate, volume ratio of 1: 1) gave 55.0 mg of a brown solid with a yield of 67%. mp: 280-282 C;

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 6293-83-0, its application will become more common.

Reference:
Patent; China Pharmaceutical University; Jiao Yu; Liu Yong; Lu Tao; Peng Qi; Chen Yadong; Tang Weifang; (36 pag.)CN110818609; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 188815-32-9,Some common heterocyclic compound, 188815-32-9, name is 3-Bromo-5-iodobenzoic acid, molecular formula is C7H4BrIO2, 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.

50.0 g (152.9 mmol) of 3-bromo-5-iodobenzoic acid was added to a 1.0 L flask and dissolved in 70 mL of chloroform under a nitrogen atmosphere.88.7 mL (1.22 mol) of thionyl chloride (SOCl2) was added, and the mixture was stirred under reflux for 18 hours. After the temperature was lowered to room temperature, the reaction solution was concentrated under reduced pressure to obtain 52.0 g (yield: 98.4%) of a yellow solid compound (Intermediate (6))

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Bromo-5-iodobenzoic acid, its application will become more common.

Reference:
Patent; WS Co.,Ltd.; Kim, Yoo Li; Koo, Cha Ryong; Oh, Yoo Jin; (30 pag.)KR101652323; (2016); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com