Author: Jessica.F

Electric Literature of 20691-72-9, These common heterocyclic compound, 20691-72-9, name is 4-Iodo-2-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.

General procedure: Ra/Ni (0.4-0.5 g) was added in small portions to a stirred solution of 6.5 mmol of the required nitro compound (4-11) in 12 mL EtOH, 12 mL 1,2-dichloroethane and 2 mL (20 mmol) hydrazine hydrate at 30 C. After completion of the Ra/Ni addition, the mixture was heated in a water bath (50 C, 60 min) and filtered through celite. The filtrate was evaporated in vacuo and crude product used for further syntheses.

Statistics shows that 4-Iodo-2-nitroaniline is playing an increasingly important role. we look forward to future research findings about 20691-72-9.

Reference:
Article; Vasic, Vesna P.; Penjisevic, Jelena Z.; Novakovic, Irena T.; Sukalovic, Vladimir V.; Andric, Deana B.; Kostic-Rajacic, Sladana V.; Journal of the Serbian Chemical Society; vol. 79; 3; (2014); p. 277 – 282;,
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Electric Literature of 4897-68-1,Some common heterocyclic compound, 4897-68-1, name is 1-Bromo-2-iodo-4-methoxybenzene, molecular formula is C7H6BrIO, 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: To a solution of Pd(OAc)2 (101 mg, 0.45 mmol ), PPh3 (354 mg, 1.35 mmol), K2CO3 (2.76 g, 20.0 mmol) in DME (30 mL) and H2O (10 mL) at room temperature under argon was added 9c (3.0 g, 11 mol). The resulting solution was stirred for 10 min, then 8 (2.83 g, 10.0 mmol) was added, and the solution was heated at reflux for 23 h and monitored by TLC. The resulting solution was cooled to room temperature, EtOAc (100 mL) was added, and the solution was washed with a saturated brine solution and water, and dried over anhydrous Na2SO4. Following evaporation of the solvent under reduced pressure, the residue was purified by chromatography on a silica gel column eluted with hexane/EtOAc (150:1) to yield 10c (2.84 g, 91%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2-iodo-4-methoxybenzene, its application will become more common.

Reference:
Article; Wu, Anhui; Xu, Daiwang; Lu, Ding; Penning, Trevor M.; Blair, Ian A.; Harvey, Ronald G.; Tetrahedron; vol. 68; 35; (2012); p. 7217 – 7233;,
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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. 620-05-3, name is (Iodomethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C7H7I

General procedure: A mixture of benzyl bromide (171 mg, 1 mmol), diphenyl disulfide (131 mg, 0.6 mmol), PPh3 (184 mg, 0.7 mmol), and [pmIm]Br21 (94 mg, 0.4 mmol) was stirred at 75 C for 1.5 h (TLC). The reaction mixture was extracted with Et2O, and the organic layer was washed with brine (2 × 5 mL) and dried (Na2SO4). Evaporation of solvent left the crude product which was purified by column chromatography over silica gel (hexane) to afford the pure product, benzyl phenyl sulfide (168 mg, 84%) as a colorless liquid. The remaining ionic liquid was washed with ether, dried under vacuum, and reused five times without appreciable loss of catalytic activity.

According to the analysis of related databases, 620-05-3, the application of this compound in the production field has become more and more popular.

Reference:
Article; Banerjee, Subhash; Adak, Laksmikanta; Ranu, Brindaban C.; Tetrahedron Letters; vol. 53; 17; (2012); p. 2149 – 2152;,
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Adding a certain compound to certain chemical reactions, such as: 1878-94-0, name is 2-(4-Iodophenoxy)acetic acid, 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 1878-94-0, SDS of cas: 1878-94-0

To (4-iodo-phenoxy)acetic acid (83.5 mg, 0.3 mmol), 3-amino-benzamide (61.3 mg, 0.45 mmol), N-(3-dimethylaminopropyl)-N’-ethyl carbodiimide HCl (EDC) (86.3 mg, 0.45 mmol) and 1-hydroxybenzotriazole (HOBt) (61.3 mg, 0.45 mmol) in DMF (3 ml) was added N,N-diisopropylethylamine, redistilled (DIPEA) (0.08 ml, 0.45 mmol). The mire was stirred overnight, and then partitioned between ethyl acetate and water. The organic phase was washed with brine, dried (MgSO4 anh), and concentrated. The residue was purified by silica gel flash column chromatography (CH2CH2:MeOH=6:1) to give 3-[2-(4-iodo-phenoxy)acetyl-amino]-benzamide as a white solid (105.1 mg, 88.4% yield). 1H-NMR (DMSO-d6) 10.22 (1H, s, NH), 8.09 (1H, s, aromatic-H), 7.94 (1H, s, NH2), 7.79 (1H, d, J=8.1 Hz, aromatic-H), 7.56-7.64 (3H, m, aromatic-H), 7.35-7.41 (2H, m, aromatic-H, NH2), 6.86 (2H, d, J=, 8.7 Hz, aromatic-H), 4.71 (2H, s, CH2).

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Reference:
Patent; KOREA RESEARCH INSTITUTE OF BIOSCIENCE AND BIOTECHNOLOGY; US2009/306078; (2009); A1;,
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Adding a certain compound to certain chemical reactions, such as: 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, 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 460-37-7, Quality Control of 1,1,1-Trifluoro-3-iodopropane

A solution of 11.3 g (26.2 mmol) of the compound from Ex. 13A in 250 ml DMF was treated with 6.10 g (57.6 mmol) of cesium carbonate and stirred for 15 min at RT.Then 11.7 g (52.3 mmol) 3,3,3-trifluoro-1-iodopropane were added, and the mixture was heated to 70 C.After 6 hours, were further 11.7 g (52.3 mmol) 3,3,3-trifluoro-1-iodopropane added.Stirring at 70 C was continued for 7 hours.After cooling to RT, most of the volatile components was (including DMF) removed on a rotary evaporator.The residue was mixed with 400 ml of ethyl acetate and washed successively with water and saturated sodium chloride solution.After drying the organic phase over anhydrous magnesium sulfate, was filtered and evaporated.The crude product was purified by MPLC on a Biotage cartridge (340 g silica gel, cyclohexane / ethyl acetate 5: 1).The product fractions were combined and evaporated.After stirring of the residue with pentane / dichloromethane (25:1).,Neuerlichem filtration and drying in a high vacuum were obtained 8.78 g (.. 63% of theory) of the title compound

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Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; HAERTER, MICHAEL; DELBECK, MARTINA; KALTHOF, BERND; LUSTIG, KLEMENS; LINDNER, NIELS; KAST, RAIMUND; WASNAIRE, PIERRE; SUESSMEIER, FRANK; (372 pag.)TW2016/7950; (2016); A;,
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Electric Literature 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.

To a solution of Pd(PPh3)2Cl2 (0.049 g, 0.079 mmol), 2-iodoisopropylbenzene (0.29 g, 1.2 mmol) in DMF (3 mL) was added 5 (0.14 g, 0.79 mmol), and triethylamine (0.33 mL, 2.4 mmol). The mixture was purged for 15 min with argon and added CuI (0.051 g, 0.27 mmol). The reaction mixture was heated overnight at 80 0C and cooled to room temperature. The resulting mixture was concentrated and purified by silica gel chromatography (hexanes/EtOAc 100:0 to 70:30 gradient) to afford the title compound as orange oil (0.089 g, 38%).[0151] 1H NMR (500 MHz, DMSO-J6): delta 1.32 (d, J = 6.9 Hz, 6H), 3.54 (qn, J = 6.9 Hz, IH), 6.69-6.70 (m, IH), 7.34 (dd, J = 7.6, 1.3 Hz, IH), 7.46 (d, J = 7.8 Hz, IH), 7.52 (dd, J = 8.0, 6.8 Hz, IH), 7.70 (d, J= 6.9 Hz, IH), 7.74-7.75 (m, IH), 12.59 (br s, IH)[0152] MS (ES+): m/z 296 (M+H)+

The synthetic route of 19099-54-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TARGEGEN INC.; WO2009/55674; (2009); A1;,
Iodide – Wikipedia,
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Synthetic Route of 202982-67-0, 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. 202982-67-0, name is 4-Chloro-3-fluoroiodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: All reactions were carried out in an 80 mL Teflon-lined stainless steel reactor equipped with a magnetic stirring bar. Typically, in a glovebox, the aryl iodides (1.0 mmol), RhI3(0.025 mmol), PPh3 (0.1 mmol), Et3N (1.2 mmol), and DMA (2 mL) were loaded into the reactor. Then, the autoclave was screwed up, charged with CO and H2 to a total pressure of 10 bar (1:1) and transferred to an oil bath preheated at 90 C, which was controlled by a Haake-D3 temperature controller. After completion of the reaction, the reactor was cooled in iced water and the gas carefully vented. The conversion and yield of the aryl iodides and arylaldehydes were determined by GC analysis using dodecane as an internal standard. For yield determination of the other products, the reaction mixture was first analyzed by GC-MS to determine the structures of the aromatic aldehyde products. Then, CH2Cl2 (5 mL) was added to the reaction mixture, after which deionized water (10 mL) was added to extract the solvent DMA for 5 times. The organic layer was dried over anhydrous Na2SO4, concentrated by rotary evaporation and finally purified by column chromatography on silica gel using n-hexane/ethyl acetate as eluent to obtain the pure products and isolated yields.

The synthetic route of 4-Chloro-3-fluoroiodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Suqing; Liu, Zhenghui; Mu, Tiancheng; Wang, Peng; Yan, Zhenzhong; Yu, Dongkun; Zhao, Xinhui; Beilstein Journal of Organic Chemistry; vol. 16; (2020); p. 645 – 656;,
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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. 7425-53-8, name is Ethyl 4-iodobutanoate, A new synthetic method of this compound is introduced below., Product Details of 7425-53-8

In a round bottom flask, compound 16 (5.0 g, 22.12 mmol) was dissolved in dry THF (50 mL) over an ice bath and sodium hydride (NaH, 1.25 g, 52.08 mmol) was added to the solution. After 20 min. stirring, ethyl 4-iodobutyrate (10.74 g, 44.24 mmol) was added to the reaction mixture. The solution was kept over ice-bath for 15 min., and then transferred to room temperature. The progress of reaction was monitored by TLC. After completion of reaction, the reaction mixture was quenched with saturated solution of NH4Cl and worked up with ethyl-acetate and washed with water. The organic layer was separated, dried over anhydrous sodium sulphate (Na2SO4) and concentrated. The crude product was then chromatographed over a column of silicagel (100-200 mesh) eluting with the ethyl acetate-hexane (2:98) to afford compound 21a as white solid. Yield: 70%; mp: 50-51C; Rf: 0.60 (30% Ethyl acetate-Hexane); IR (KBr, numax/cm-1): 2957, 1729, 1673, 1599, 1261, 1026, 830, 741; 1H NMR (CDCl3, 500 MHz, delta ppm): 1.21 (t, J = 7.0 Hz, 3H, CH3), 1.25-1.65 (m, 2H, CH2), 1.83 (d, J = 5.0 Hz, 1H, CH2), 2.16 (t, J = 5.5 Hz, 1H, CH2), 2.27-2.32 (m, 2H, CH2), 3.81 (s, 3H. OCH3). 4.08 (q, J = 7.0 Hz, 2H, OCH2), 4.49 (t, J = 7.0 Hz, 1H, CH), 6.84-6.87 (m, 2H, ArH), 7.17-7.20 (m, 1H, ArH), 7.26-7.30 (m, 4H, ArH), 7.93-7.96 (m, 2H, ArH); 13C NMR (CDCl3, 125 MHz, delta ppm): 14.2, 23.1, 33.4, 34.2, 53.1, 55.4, 60.2, 113.7 (2xC), 127.0, 128.1 (2xC), 128.9 (2xC), 129.7, 130.9 (2xC), 139.7, 163.3, 173.4, 198.0; EIMS (C21H24O4): m/z = 341.2 [M+H]+.

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; Bawankule, Dnyaneshwar U.; Gupta, Atul; Imran Ahamad, Mohd.; John, Aijaz A; Khan, Feroz; Luqman, Suaib; Prakash, Ravi; Singh, Divya; Wani, Zahoor; Yadav, Deepika; Bioorganic and medicinal chemistry letters; (2020);,
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Adding a certain compound to certain chemical reactions, such as: 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, 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 608-28-6, Application In Synthesis of 2-Iodo-1,3-dimethylbenzene

To a so?ution of 5-(4455- tetramethy-1 32-dioxaboroan-2-y)-1 H-benzo[djimidazo-2(3H)-one (ntermediate 28, 100mg 0.38 mmo), potassium phosphate (204 mg, 0.96 mmo), and PdC2(dtbpf) (13 mg0.019 rnrno) in 4:1 dioxane:water (2.0 mL) was added 2,6-dimethyhodobenzene at once(178 mg 0.77 mmo). The mixture was degassed with nitrogen for 10 minutes and then heated at 100 C for 16 h, After cooHg to rt, the reaction mixture was duted wfth water and extracted w[th EtOAc (x 3). The combned organc extracts were dried (Na2SO4), fUtered and concentrated under reduced pressure. Purficaton (FCC, SO2; 0 – 100% EtOAc/hexanes) afforded the tWe compound as a wh[te sod (22 mg, 24% yed). MS(ES): mass cacd. for C15H14N20, 238.1; m/zfound, 239.0 [M+H]. 1H NMR (400 MHz, CD3OD) 5 713- 7.02 (m, 4H), 6.86- 6.80 (m, 1H), 6.76 (dd, J= 80, 1.4 Hz, 1 H), 2.00 (s, 6H).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; RAVULA, Suchitra; SWANSON, Devin M.; SAVALL, Bradley M.; AMERIKS, Michael K.; (250 pag.)WO2016/176449; (2016); A1;,
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Electric Literature of 401-81-0, A common heterocyclic compound, 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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: To a solution of aryl iodide (10 mmol, 1.0 equiv.) in THF (10 mL, 1.0 M) was added 2-propyn-1-ol (1.24 mL, 1.2 equiv.), diisopropylamine (1.68 mL, 1.2 equiv.), PdCl2(PPh3)2 (0.3 mmol, 3 mol%) andCuI (0.5 mmol, 5 mol%). The resulting solution changed colour from yellow to orange and finallybrown in two minutes. The reaction mixture was heated at 50 C and stirred until completeconsumption of the aryl iodide was observed (tlc, 2 h). After filtering the crude material over a padof silica (5 g) and evaporation of the solvent the crude material (1H-NMR) was purified by silica column chromatography (eluent 10% EtOAc in pentanes, Rf = 0.41). After removal of the volatiles,the desired hydroxyl product was typically isolated as yellow oil with a purity > 98% (by 1H-NMR)and was used directly in the next step. Copies of NMR spectra are provided in the electronicsupplementary information.

The synthetic route of 401-81-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Donnelly, Kian; Zhang, Huan; Baumann, Marcus; Molecules; vol. 24; 20; (2019);,
Iodide – Wikipedia,
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