Month: June 2021

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).

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; KOREA RESEARCH INSTITUTE OF BIOSCIENCE AND BIOTECHNOLOGY; US2009/306078; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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

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; 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;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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;,
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. 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);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 573764-31-5,Some common heterocyclic compound, 573764-31-5, name is 4-Chloro-3-iodoaniline, molecular formula is C6H5ClIN, 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.

A mixture of compound 3 (5 mmol), 4,4,4′,4′,5,5,5′,5′-Octamethyl-2,2- bi(1,3,2-dioxaborolane) (10 mmol), KOAc (10 mmol), PdCl2(dppf) (0.1 mmol) in DMF (20 mL) was stirred at 95 °C for 2 h under Ar. The reaction mixture was filtered through celite. The filtrate was concentrated in vacuo and then extracted with CH2Cl2. The organic layer was evaporated to give a residue, which was purified by chromatography (petroleum ether/CH2Cl2, 10:1) to afford a white solid, yield 50percent. 1H NMR (400 MHz, DMSO-d6) delta 7.10 (d, J = 8.5 Hz, 1H), 6.97 (d, J = 2.9 Hz, 1H), 6.70 (dd, J = 8.5, 2.9 Hz, 1H), 5.32 (s, 2H), 1.38 (s, 12H). 13C NMR (101 MHz, DMSO) delta 147.40, 129.97, 124.63, 121.85, 118.00, 84.08 (2C), 25.08 (4CH3).

The synthetic route of 573764-31-5 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Wenlu; Sun, Qinsheng; Song, Lu; Gao, Chunmei; Liu, Feng; Chen, Yuzong; Jiang, Yuyang; European Journal of Medicinal Chemistry; vol. 141; (2017); p. 721 – 733;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 74-88-4, 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 74-88-4 as follows.

General procedure: Iodomethane (1.606mmol) was added to a stirred solution of 1a (0.143mmol) and anhydrous potassium carbonate (0.352mmol) in dry CH2Cl2(2 mL), in an N2atmosphere at 55 C. The mixture was stirred for 24h and iodomethane (1.606mmol) was added once again and stirred for another 24h. After 48h, the reaction mixture was diluted in water (50 mL) and the aqueous phase was extracted with dichloromethane (3 x 50 mL). The resulting organic phase was washed with brine, dried over Na2SO4, filtered and evaporated. In order to produce a white solid, the organic phase was purified by silica gel chromatography using a gradient elution of C6H12/CH2Cl2(Yield: 24%).

According to the analysis of related databases, 74-88-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Cargnin, Simone Tasca; Staudt, Andressa Finkler; Medeiros, Patricia; de Medeiros Sol Sol, Daniel; de Azevedo dos Santos, Ana Paula; Zanchi, Fernando Berton; Gosmann, Grace; Puyet, Antonio; Garcia Teles, Carolina Bioni; Gnoatto, Simone Baggio; Bioorganic and Medicinal Chemistry Letters; vol. 28; 3; (2018); p. 265 – 272;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. category: iodides-buliding-blocks

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