Month: March 2021

Application of 696-41-3, The chemical industry reduces the impact on the environment during synthesis 696-41-3, name is 3-Iodobenzaldehyde, I believe this compound will play a more active role in future production and life.

General procedure: BiCl3-MK10 catalyst (0.1 g) was added to a mixture of indole (2 mmol) and aldehyde (1 mmol), and the mixture was ground in a mortar with a pestle at room temperature. After completion of the reaction (tested by thin-layer chromatography, TLC), ethyl acetate was added and the insoluble catalyst was removed by filtration. The filtrate was dried over anhydrous Na2SO4. The solvent was evaporated under vacuum to furnish the product. All the products were characterized by GC-MS, and selected compounds were characterized by 1H and 13C NMR. NMR data for three representative compounds are given below.

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, 3-Iodobenzaldehyde, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ravi; Krishnakumar; Swaminathan; Research on Chemical Intermediates; vol. 41; 8; (2015); p. 5353 – 5364;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 41860-64-4, These common heterocyclic compound, 41860-64-4, name is 4-Fluoro-2-iodo-1-nitrobenzene, 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.

A. 5-fluoro-4′-methylsulfinyl-2-nitrobiphenylamine 2-Iodo-4-fluoronitrobenzene (0.2 mole) and p-methylsulfinylaniline (0.2 mole) are refluxed in dry dimethylformamide (300 ml.) containing copper powder (5 gm.) and some powdered potassium carbonate (20 gm.) under nitrogen for 18 hours. The solution is filtered and the organics washed with water (6 * 100 ml.) in benzene (600 ml.). The benzene layer is extracted with 2.5 N HCl (7 * 200 ml.) and the acid layer poured onto powdered sodium bicarbonate. The basic solution is extracted with benzene (6 * 200 ml.), the benzene layer washed with water (3 * 100 ml.), separated, dried (MgSO4) and filtered. Evaporation of the solvent followed by chromatography on a 2 in. * 24 in. column of silica-gel (Baker) eluted with various proportions of benzene-hexane mixtures gives pure 5-fluoro-4′-methylsulfinyl-2-nitrobiphenylamine.

The synthetic route of 41860-64-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merck & Co., Inc.; US3954852; (1976); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 2142-70-3, name is 1-(2-Iodophenyl)ethanone, 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 2142-70-3, Formula: C8H7IO

Example 4 -Cyclohexyl-3 -hydroxy- l-(2-iodophenyl)propan-l -one[0173] To a solution of diisopropylamine (1.6 mL, 1 1.1 mmol) in THF (38 mL) at 0 C was added w-BuLi (4.1 mL, 10.2 mmol) under an atmosphere of N2. After 30 min the solution was cooled to -30 C and a solution of l-(2-iodophenyl)ethanone (2.27 g, 9.23 mmol) in THF (6 mL) was added dropwise to the mixture and was stirred for 45 min at -30 C. The mixture was cooled to -78 C and cyclohexylcarboxaldehyde (1.2 mL, 9.69 mmol) was added dropwise and the mixture was allowed to warm to -40 C over 2 h. The reaction was quenched by the addition of saturated aqueous NH4C1. The aqueous layer was extracted with EtOAc (2 x 50 mL). The combined organic layers were washed with brine, dried (Na2S04), filtered and concentrated. The residue was purified by flash column chromatography to afford the title compound as yellow oil (2.56 g, 78%). H NMR: 1.02-1.27 (m, 4H), 1.41-1.49 (m, 1H), 1.66-1.76 (m, 4H), 1.89 (d, 1H, J= 12.4 Hz), 2.88 (d, 1H, J = 3.2 Hz), 2.98 (dd, 1H, J = 9.2 Hz, 17.2 Hz), 3.13 (dd, 1H, J = 2.0 Hz, 17.2 Hz), 3.99-4.01 (m, 1H), 7.1 1-7.15 (m, 1H), 7.42 (d, 2H, J= 4.4 Hz), 7.93 (d, 1H, J= 8.0 Hz).

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; NEWLINK GENETICKS CORPORATION; MAUTINO, Mario; KUMAR, Sanjeev; WALDO, Jesse; JAIPURI, Firoz; KESHARWANI, Tanay; WO2012/142237; (2012); A1;,
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. 29289-13-2, name is 2-Iodo-4-methylaniline, This compound has unique chemical properties. The synthetic route is as follows., name: 2-Iodo-4-methylaniline

General procedure: A mixture of 2-halobenzenamine (1.0 mmol), isothiocyanate (1.2 mmol), Et3N (2.0 mmol) and MCM-41-2N-CuSO4 (0.0025 mmol) in DMSO (2 mL) was stirred under an air atmosphere at 80 C for 5-24 h. After completion of the reaction as indicated by TLC, the mixture was cooled to room temperature. The solution was diluted with ethyl acetate (30 mL ) and filtered. The catalyst was washed with ethyl acetate (2 ¡Á 5 mL) and Et2O (2 ¡Á 5 mL) and reused in the next run. The organic layer was washed with water (2 ¡Á 10 mL) and dried over anhydrous Na2SO4. After evaporating under vacuum, the residue was purified by flash chromatography on silica gel (petroleum/ethyl acetate = 10:1 to 4:1) to provide the corresponding pure product 3.

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 29289-13-2.

Reference:
Article; Xiao, Ruian; Hao, Wenyan; Ai, Jinting; Cai, Ming-Zhong; Journal of Organometallic Chemistry; vol. 705; (2012); p. 44 – 50;,
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. 52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, A new synthetic method of this compound is introduced below., name: 5-Fluoro-2-iodobenzoic acid

Intermediates 8 and 9: 5-Fluoro-2-(2H-1,2,3-triazol-2-yl)benzoic acid (Intermediate 8) and 5-Fluoro-2-(1H-1,2,3-triazol-1-yl)benzoic acid (Intermediate 9) To a solution of 2H-1,2,3-triazole (CAS number 288-36-8; 4.0 g, 57.97 mmol) in DMF (14.0 ml) was added cesium carbonate (18.84 g, 57.97 mmol), trans-1-N,2-N-dimethylcyclohexane-1,2-diamine (0.510 g, 5.797 mmol), copper(I) iodide (0.276 g, 1.449 mmol) and 5-fluoro-2-iodobenzoic acid (CAS number 52548-63-7; 7.71 g, 28.98 mmol) at 0-10 C. The resulting reaction mixture was then heated with microwave irradiation at 125 C. for 15 hours with stirring. The reaction mass was poured into water and the product was extracted into ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate and concentrated in vacuo. This was then purified by column chromatography (silica, 0-3% methanol/DCM) to obtain 5-fluoro-2-(2H-1,2,3-triazol-2-yl)benzoic acid (Intermediate 8) (also commercially available CAS number 1186050-64-5) and crude 5-fluoro-2-(1H-1,2,3-triazol-1-yl)benzoic acid (Intermediate 9). The crude compound (Intermediate 9) obtained was further purified by column chromatography (silica, 0-3% methanol/DCM) and then by reverse phase preparative HPLC (eluted with acetonitrile/water with 0.1% ammonia) to afford the title compound.

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; Takeda Pharmaceutical Company Limited; Fieldhouse, Charlotte; Glen, Angela; Maine, Stephanie; Fujimoto, Tatsuhiko; Robinson, John Stephen; US2015/232460; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

2265-91-0, name is 1,3-Difluoro-5-iodobenzene, 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. COA of Formula: C6H3F2I

General procedure: A Schlenk tube with a magnetic stir bar was charged with Pd(OAc)2 (10 mol%, 0.0056 g), AgOTf (1.1 equiv., 0.0707 g), TBAB (20 mol%, 0.0161g), 2-phenylpyridine N-oxides 1 (0.25 mmol), iodobenzene and its derivatives 2 (0.375 mmol) and H2O (1 mL). The resulting solution was stirred at 100C for 12 h. The resulting organic layer was extracted with trichloromethane, treated with Na2SO4 and concentrated in vacuo. The product was isolated by short column chromatography using ethyl acetate and methanol as eluent.

The synthetic route of 2265-91-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Wei; Li, Zhengkai; Zhang, Yihan; Yang, Li; Zhou, Xiangge; Synthetic Communications; vol. 47; 8; (2017); p. 793 – 802;,
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. 13421-00-6, name is 5-Chloro-2-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 5-Chloro-2-iodobenzoic acid

A solution of 5-chloro-2-iodobenzoic acid (3.0 g, 10.62 mmol), SOC12 (12 mL) and DMF (0.6 mL) was gently warmed with a heat gun until the mixture becamehomogeneous (15 mm). The solution was maintained at 23C for additional 30 mm and then the solution was concentrated. MeOH (24 mL) was added to the crude residue and the solution was maintained at 23C for 30 mm. The solution was concentrated and the residue was purified by flash chromatography on Biotage silica gel cartridge (cyclohexane to cyclohexane : EtOAc = 85 : 15) to afford methyl 5-chloro-2-iodobenzoate (3.02 g, 10.20 mmol, 96%).UPLC-MS: 1.17 mm, 296.6 [M+H]+, method 12.

The synthetic route of 13421-00-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CHIESI FARMACEUTICI S.P.A.; BIAGETTI, Matteo; CAPELLI, Anna Maria; ACCETTA, Alessandro; CARZANIGA, Laura; WO2015/91685; (2015); 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. 627-32-7, name is 3-Iodo-1-propanol, A new synthetic method of this compound is introduced below., SDS of cas: 627-32-7

5 g of E-oct-4-ene-1,8-dioic acid was added to 25 mL of thionyl chloride, and the mixture was heated under reflux for 3 hours.After the reaction was cooled to room temperature, spin dry and dissolved in 50 mL of dichloromethane.Then, it was slowly added dropwise to 100 mL of tetrahydrofuran in which 33.5 g of 3-iodopropanol was dissolved at about 0 C, and the reaction was carried out at 0 C for 24 hours after completion of the dropwise addition.The reaction was completely detected by HPLC, and 50 mL of 1 M KOH was added.Sodium quenching reaction.After liquid separation, the organic phase was dried over anhydrous sodium sulfate.The compound E-oct-4-ene-1,8-dioic acid bis(3-iodopropyl) ester 12.1 g (yield 81.6%) was obtained as a pale yellow oily liquid, purity 95.3%.

The synthetic route of 627-32-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wuhan Jianuokang Pharmaceutical Co., Ltd.; Wei Wenguo; Wang Yajun; (13 pag.)CN108503564; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 31827-94-8, 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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To 2.50 g (7.69 mmol) 2-bromo-1 -(4-iodo-phenyl)-ethanone in 30 mL ACN are added 1 .90 g (23.1 mmol) 4-methylimidazole and the mixture is stirred at rt for 48 h. After that time, the solvent is evaporated and the residue is taken up in EtOAc. The mixture is washed with water and brine (2x) and the organic layer is dried over magnesium sulphate. The solvent is evaporated and the residue is recrystallized from diethyl ether to yield the desired product.C12H11 IN2O (M = 326.13 g/mol)ESI-MS: 327 [M+H]+

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, 2-Bromo-1-(4-iodophenyl)ethanone, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; ROTH, Gerald Juergen; FLECK, Martin; NEUBAUER, Heike; NOSSE, Bernd; WO2012/32014; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 620621-48-9, A common heterocyclic compound, 620621-48-9, name is Methyl 2-chloro-5-iodobenzoate, molecular formula is C8H6ClIO2, 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.

A mixture of 2-chloro-5-iodo-benzoic acid methyl ester (3.5 g, 12 mmol), dichlorobis (triphenylphosphino) palladium (II) (0. 04 g, 0.06 mmol), triphenylphosphine (0.06 g, 0.24 mmol), copper iodide (0.05 g, 0.24 mmol), (trimethylsilyl) acetylene (1.9 g, 19.2 mmol) in triethylamine (40 mL) was heated at reflux for 12h. The mixture was concentrated in vacuo, diluted with ethyl acetate (150 mL) and washed sequentially with 10% aqueous citric acid, water, and brine. The organic solution was dried, filtered and concentrated in vacuo to afford the title compound (3.14 g).

The synthetic route of 620621-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PFIZER PRODUCTS INC.; WO2004/99146; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com