Author: Jessica.F

Related Products of 13421-13-1, 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. 13421-13-1, name is 4-Chloro-2-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: DMF (2 drops) and oxalyl chloride (180 muL, 2.12 mmol) were added to a suspension of 4-chloro-2-iodobenzoic acid (0.400 g, 1.42mmol) in toluene (5 mL). After the acid had dissolved and evolution of gas had ceased, the mixture was concentrated under vacuum to afford the crude acyl chloride, which was used without further purification.To a soln of this crude acyl chloride in CH2Cl2 (6 mL) was added a soln of Et3N (592 muL, 4.25 mmol) and aniline (129 muL,1.42 mmol) in CH2Cl2 (6 mL). The mixture was stirred for 1 h and then sat. aq NH4Cl soln (5 mL) was added. The aq layer was extracted with CH2Cl2 (3 ¡Á 5 mL) and the combined organic layers dried (Na2SO4) and evaporated. The crude residue was purified by flash chromatography (hexanes-EtOAc, 90:10 to 85:15), to afford 5e (400 mg, 79%) as a white solid. Mp 172-173 C. IR (film): 1653 (s), 1600 (s) cm-1. 1H NMR (300.13 MHz, acetone-d6): delta = 7.18 (t, J = 7.4 Hz, 1 H), 7.41 (t, J = 7.8 Hz, 2 H), 7.57 (s, 1 H), 7.83 (d, J = 7.8 Hz, 2 H), 8.00(s, 1 H), 9.55 (s, 1 H). 13C NMR (75.47 MHz, acetone-d6): delta = 93.8 (C), 120.6 (2 ¡Á CH), 124.9 (CH), 129.1 (CH), 129.6 (2 ¡Á CH), 130.0 (CH), 136.0 (C), 139.5 (CH), 139.9 (C), 143.0 (C), 167.4 (C). MS (EI): m/z (%) = 359 (7) [37Cl, M]+, 357 (20) [35Cl, M]+, 267 (25), 265 (base). HRMS (EI): m/z [M]+ calcd for C13H935ClINO: 356.9417; found: 356.9423; m/z [M]+ calcd for C13H937ClINO: 358.9388; found: 358.9385.

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

Reference:
Article; Madich, Youssef; Denis, J.Gabriel; Ortega, Aitor; Martinez, Claudio; Matrane, Abdellatif; Belachemi, Larbi; De Lera, Angel R.; Alvarez, Rosana; Aurrecoechea, Jose M.; Synthesis; vol. 45; 14; (2013); p. 2009 – 2017;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 3718-88-5,Some common heterocyclic compound, 3718-88-5, name is 3-Iodobenzylamine hydrochloride, molecular formula is C7H9ClIN, 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 150: Synthesis of 4-Chloro-6-[3-(3-dimethylamino-propylamino)- benzylamino]-2//-phthalazin-l-one hydroformate; (3-Iodo-benzyl)-carbamic acid tert-butyl ester; A mixture of 3-iodobenzylamine hydrochloride (3g, 11.131 mmol), CH2Cl2(6OmL) and triethylamine (3.ImL, 22.263 mmol) was stirred at room temperature. Boc- anhydride (2.6Og, 11.913 mmol) was added and the reaction stirred at room temperature for Ih. The reaction was poured onto water, extracted with CH2Cl2 and dried (Na2SO4). Preparatory HPLC afforded (3-iodo-benzyl)-carbamic acid tert-butyl ester (3.494g) as a white solid, m/z (M+l) 333.84.

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

Reference:
Patent; FOREST LABORATORIES HOLDINGS LIMITED; WO2008/61108; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 375-80-4, name is 1,6-Diiodoperfluorohexane, 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 375-80-4, Computed Properties of C6F12I2

General procedure: In a typical procedure (IC2F4)2 (45.40g, 0.1mol) was dissolved in 100mL of acetonitrile and 200mL of water in a 500-mL round-bottomed flask. The solution was made basic with NaHCO3 (30.00g, 0.36mol) and then fresh Na2S2O4 (50.00g 0.28mmol, the ratio is 1:2.8) was slowly added with good stirring at 22C. After 20h, fluorine-19 NMR spectroscopy indicated the reaction was complete by disappearance of the -CF2I signal. The solution (NaSO2C2F4)2 and other byproducts are light yellow.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,6-Diiodoperfluorohexane, and friends who are interested can also refer to it.

Reference:
Article; Mei, Hua; Desmarteau, Darryl D.; Journal of Fluorine Chemistry; vol. 160; (2014); p. 12 – 15;,
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. 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