Month: March 2021

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. 450412-28-9, name is 1-Bromo-3-chloro-2-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C6H3BrClI

A 500-mL round-bottom flask under N2 atmosphere was charged sequentially with Pd(Ph3P)4, l-bromo-3-fluoro-2-iodobenzene (10 g, 0.032 mol) in toluene (80 mL), 2N aqueous sodium carbonate (55 mL) and 3-methylphenylboronic acid (5.16 g, 0.032mol) dissolved in ethanol (40 mL). This mixture was heated at reflux under N2 for 12 h and cooled to rt. The mixture was partitioned between water and EtOAc. The combined organic layers were washed with brine, dried over MgSO4, and concentrated. The residue was purified by column chromatography to give 6-bromo-2-chloro-3′-methyl-biphenyl (6 g, 67%). 1H NMR (400MHz, CD3OD): 6.90-7.00 (t, 2H), 7.14-7.24 (m, 2H), 7.26-7.33 (t, IH), 7.44-7.50 (d, IH), 7.58-7.62 (d, IH); MS (E/Z): 281 (M+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 450412-28-9.

Reference:
Patent; VITAE PHARMACEUTICALS, INC.; WO2007/117560; (2007); A2;,
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. 2468-56-6, name is 6-Iodohex-1-yne belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 6-Iodohex-1-yne

At -40C, a solution of lithium bis(trimethylsilyl)amide 1 M in tetrahydrofuran (38.9 mmol, 38.9 mL, 2.2 eq) was added dropwise to a solution of glutarimide (2.0 g, 17.7 mmol, 1 .0 eq) in tetrahydrofuran (30 mL). The iodoalkane (53.1 mmol, 3.0 eq) was immediately added. After 15 minutes at -40C, the mixture was allowed to warm up and the mixture was stirred at room temperature for 18 hours. The reaction was quenched with a saturated solution of ammonium chloride (10 mL) and the aqueous phase was extracted with methylene chloride (3 x 20 mL). The combined organic phases were dried over magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by flash chromatography using cyclohexane and ethyl acetate (1 00/0 to 0/100) to afford the expected compound. General procedure B: alkylation with LDA; 3-hex-5-ynyl-piperidine-2,6-dione was prepared according to General Procedure A using glutarimide (2.0 g, 17.7 mmol) and 6-iodo-J-hexyne (5.6 mL. 42.4 mmol). The expected compound was isolated as orange oil that solidified during storage with 17% yield (570 mg).

The synthetic route of 2468-56-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITY OF SOUTHERN CALIFORNIA; PRESTWICK CHEMICAL, SAS; LADNER, Robert D.; GIETHLEN, Bruno; WO2014/107622; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 31827-94-8, 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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, This compound has unique chemical properties. The synthetic route is as follows.

Into a 25 mL eggplant-shaped flask was added 1 mmol of N-(4-trifluoromethylphenyl)thiourea.1.05 mmol alpha-bromo-4-iodophenone,Add 10mL of ethanol to dissolve, add 1.5mmoL of triethylamine,Reflux reaction. After TLC tracks the reaction,The temperature of the reaction solution was lowered to room temperature, and the solvent was distilled off under reduced pressure.Column chromatography of the residue (eluent: petroleum ether-ethyl acetate) yields the target compound,White solid, yield 82%.

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

Reference:
Patent; Shanghai Pharmaceutical Industry Institute; East China University of Science and Technology; Chen Daijie; Xu Xiaoyong; Shao Lei; Li Zhong; Dong Xiaojing; Hou Shuang; Zhang Junliang; Wang Rong; (81 pag.)CN107629022; (2018); 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

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 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

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

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 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

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