Month: April 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. 32024-15-0, name is 3-Iodo-4,5-dimethoxybenzaldehyde, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 3-Iodo-4,5-dimethoxybenzaldehyde

3, 4-dimethoxy-5-iodo-benzaladehyde (2.92 g, 10 mmol) wasdissolved in minimal EtOH and stirred in an ice bath. After the entire solid had dissolved NaBH4 (3.4 g,~10 mmol) was added to the mixture. The progress was monitored by HPLC. After, 1.5 hours thecomplete reaction mixture was concentrated under vacuum to half its volume and poured into aseparating funnel containing water. Aqueous layer was extracted three times with DCM. It was thenconcentrated to give the final product as yellow oil (2.79 g, 9.5 mmol). 1H NMR (300 MHz, DMSO-d6): 7.40 – 7.27 (m, 1H), 7.02 (d, J = 1.7 Hz, 1H), 4.53 (s, 2H), 3.87 (s, 3H), 3.77 (s, 3H). UV-Vis: 214.7, 285.1nm.

According to the analysis of related databases, 32024-15-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Maresh, Justin J.; Ralko, Arthur A.; Speltz, Tom E.; Burke, James L.; Murphy, Casey M.; Gaskell, Zachary; Girel, Joann K.; Terranova, Erin; Richtscheidt, Conrad; Krzeszowiec, Mark; Synlett; vol. 25; 20; (2014); p. 2891 – 2894;,
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. 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane

In a 20 liter reaction vessel, 1500 g (3.16 mol) of 1H, 1H, 2H, 2H-perfluorohexylethyl iodide and 3 L of dimethylformamide were added, and 230 g (3.5 mol) of sodium azide was added. The mixture was stirred at room temperature for 3 h, GC showed complete conversion, selectivity 99%, water 3 L, allowed to stand, layered, the aqueous layer was washed three times with methyl tert-butyl ether,The three washed organic layers were washed three times with brine to give crude 1H, 1H, 2H, 2H-perfluorooctyl azide containing methyl tert-butyl ether.

According to the analysis of related databases, 2043-57-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Juhua Group Technology Center; Wang Zhiguang; Jiang Yun; (6 pag.)CN106278921; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 689291-89-2, name is 5-Bromo-2-iodobenzaldehyde, 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 689291-89-2, Quality Control of 5-Bromo-2-iodobenzaldehyde

To an ice-cold solution of 2,2,5, 5-tetramethyldihydrofuran-3-one (0.388g, 2.73mmoles) in anhydrous 1 ,2-diotamethoxyethane (5ml) is added sodium methoxide (0.177g, 3.27mmoles) in one portion. The reaction mixture is stirred for 5 minutes at this temperature, followed by the dropwise addition of 5-bromo-2-iodo-benzaldehyde (0.85Og, 2.73mmoles) as a solution in 1 ,2-dimethoxyethane (5ml). The reaction mixture is further stirred at O0C for 30 minutes, then at ambient temperature for a 1 hour. After partitioning between 1 M hydrochloric acid and dichloromethane, the organic phase is separated, and the aqueous phase is extracted again with additional dichloromethane. All organics are combined then concentrated in vacuo to afford 4-[1-(5-bromo-2-iodophenyl)methyliotadene]-2,2,5,5-tetramethyldihydrofuran-3-one(1.18g) as a yellow gum.

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; SYNGENTA LIMITED; SCUTT, James Nicholas; WO2010/136431; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 83171-49-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 83171-49-7 name is 3-Chloro-5-iodoaniline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: The corresponding pyrazinoic acid (5.0 mmol) was dispersed in dry toluene (20 mL) and mixed with 1.5eq. of thionyl chloride (0.55 mL, 7.5 mmol). The reaction mixture was heated to reflux for approximately 1 h. Next, the excess of thionyl chloride was removed by repeated evaporation with dry toluene under vacuum.The crude acyl chloride was dissolved in dry acetone(20 mL) and added drop-wise to a stirred solution of the corresponding aniline (5.0 mmol) with triethylamine(5.0 mmol) in dry acetone (30 mL). The reaction mixture was stirred at ambient temperature for up to 6 h. The completion of the reaction was monitored by TLC (eluent: hexane/ethyl acetate; r =2 : 1). The crude product adsorbed on silica gel by solvent evaporation was purified by flash chromatography(hexane/ethyl acetate gradient elution).The analytical data of the prepared compounds were fully consistent with the proposed structures and are available in the Supplementary Data.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Chloro-5-iodoaniline, and friends who are interested can also refer to it.

Reference:
Article; Zitko, Jan; Barbora, Servusova-Vanaskova; Paterova, Pavla; Navratilova, Lucie; Trejtnar, Frantisek; Kunes, Jiri; Dolezal, Martin; Chemical Papers; vol. 70; 5; (2016); p. 649 – 657;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 98-61-3, A common heterocyclic compound, 98-61-3, name is 4-Iodobenzenesulfonyl chloride, molecular formula is C6H4ClIO2S, 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: C5-Arylated Furans; General Procedure To a 25-mL oven-dried Schlenk tube, arenesulfonyl chloride (1.5-2 mmol), furan derivative (1 mmol), Li2CO3 (0.222 g, 3 mmol), 1,4-dioxane (2 mL) and PdCl2(MeCN)2 (12.9 mg, 0.05 mmol) wereadded successively. The mixture was evacuated by vacuum-argoncycles (5 ) and stirred at 140 C (oil bath temperature) for 20-72 h(see tables and schemes). After cooling the reaction at r.t. and con-centration, the crude mixture was purified by column chromatogra-phy (silica gel) to afford the C5-arylated furans.

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; Beladhria, Anissa; Yuan, Kedong; Ben Ammar, Hamed; Soule, Jean-Francois; Ben Salem, Ridha; Doucet, Henri; Synthesis; vol. 46; 18; (2014); p. 2515 – 2523;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 21740-00-1, name is 5-Bromo-2-iodobenzoic 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 21740-00-1, Computed Properties of C7H4BrIO2

General procedure: A sealed tube was charged with CuCl (0.02 mmol), BFMO (0.02 mmol), N-protected N-alkenylhydrazine (2.0 mmol), 2-iodobenzoic acid (2.4 mmol), and K2CO3 (4 mmol). The tube was evacuated and backfilled with argon three times before anhydrous DMSO (4.0 mL) was added via syringe (NOTE: for liquid substrates, they were added into the tube via syringe after the tube was backfilled with argon). The mixture was sealed and stirred at 80 C for 24 h. The mixture was diluted with EtOAc, washed with water, dried over anhydrous sodium sulfate, and filtrated. The filtrate was concentrated in vacuo and the residue was treated with 4M HCl/1,4-dioxane (1.2 mL) at 80 C. After the starting material was completely consumed, the solution was cooled and diluted with EtOAc. The resultant mixture was washed with water and dried over anhydrous sodium sulfate. After the solution was concentratedin vacuo, the residue was purified by flash chromatography to afford the corresponding indole.

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:
Article; Wei, Quanpeng; Wang, Yunhan; Zhao, Jinlong; Zhang, Xiaojing; Ma, Dawei; Tetrahedron; vol. 76; 1; (2020);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 124700-41-0, These common heterocyclic compound, 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid, 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.

Preparation 29 Ethyl 3-(2-fluoro-5-iodophenyl)-3-oxopropanoate To a stirred solution of 5.32 g of 2-fluoro-5-iodobenzoic acid from Preparation No. 28 in 20 mL of THF, under argon, is added 3.9 g of carbonyldiimidazole. In a separate flask, 2.8 mL of chlorotrimethylsilane is added to a mixture of 3.74 g of potassium ethyl malonate in 20 mL of acetonitrile. The mixture is stirred under argon for 18 h, then cooled to 0 C. for the dropwise addition of 6.6 mL of DBU. The mixture is stirred for 3 h at 0 C., then the solution of acyl imidazolide prepared above is added via cannula. After 2 h, the mixture is partitioned between ether and excess dilute HCl, and the organic phase is washed with dilute HCl and brine and dried (MgSO4). Removal of the solvent under reduced pressure left a colorless oil, which is flash chromatographed on silica using 10% ethyl acetate in hexane to provide 5.07 g of the title compound as dense pinkish prisms. Physical properties as follows: 1H NMR (CDCl3) delta1.34, 4.27, 5.82, 6.89, 7.7, 8.2 ppm; IR 1624, 1485, 1419, 1245, 1193, 1070, 1028, 813 cm-1.

Statistics shows that 2-Fluoro-5-iodobenzoic acid is playing an increasingly important role. we look forward to future research findings about 124700-41-0.

Reference:
Patent; Pharmacia & Upjohn Company; US6248739; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 16355-92-3, These common heterocyclic compound, 16355-92-3, name is 1,10-Diiododecane, 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.

Intermediate 1 (300 mg, 0.67 mmol), 1 ,10-diiododecane (600 mg, 1.5 mmol), 1 M aqueous sodium hydroxide (1.5 ml, 1.5 mmol), tetra-n-butylamonium iodide (27 mg, 0.072 mmol) and water (2 ml) were charged into a 5 ml Biotage microwave vial. The mixture was then irradiated at 1400C for 5 min. The resulting orange solution was extracted with EtOAc and the combined EtOAc fractions were reduced to afford an orange gum. Purification was achieved via column chromatography (loaded onto diatomaceous earth) using 0-14% step gradient of EtOAc in cyclohexane (2% steps) as eluent, followed by 100% cyclohexane, followed by 30% EtOAc in cyclohexane to afford the product as a colorless gum.Yield: 272 mg (57%)LC-MS (Method 3): Rt 5.57 min, m/z 711 [MH+]

The synthetic route of 16355-92-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ARGENTA DISCOVERY LTD.; WO2007/42815; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 455-13-0, 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. 455-13-0, name is 4-Iodobenzotrifluoride belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

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.

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

Reference:
Article; Donnelly, Kian; Zhang, Huan; Baumann, Marcus; Molecules; vol. 24; 20; (2019);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 19099-54-8, 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. 19099-54-8, name is 1-Iodo-2-isopropylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of N,7-[(benzothiazol-2-yl)-9,9-diethylfluoren-2-yl)-N-(2,6-diisopropylphenyl)amine (Example 19; 4.24 g, 8 mmol), 2-isopropyl iodobenzene (12.3 g, 50 mmol), 18-crown-6 (0.169 g), copper powder (1 g, 15.7 mmol) and potassium carbonate (4.41 g, 32 mmol) was kept at 240 C. for 4 hours under nitrogen, cooled, diluted with toluene and filtered. The filtrate was washed with water, dried and concentrated. The residue (15.32 g) was chromatographed over silica gel. The column was eluted with 1:1 toluene to get the product, and the product was crystallized from a mixture of isopropanol and toluene, 3.85 g (74%), m.p. 259.3-262.9 C. Mass spec: m/z 648 (M+). Anal. Calcd. for C45H48N2S: C, 83.29; H, 7.46; N, 4.32 and S, 4.94%. Found: C, 83.33; H, 7.45; N, 4.31 and S, 4.96%. 1H NMR (CDCl3) delta ppm: 0.29, 0.32 (2t, 6H, 7.28, 7.36 Hz), 0.75 (broad envelope 6H), 1.18 (broad, 12H), 1.90 (m, 2H), 2.08 (m, 2H), 3.20 (broad s?, 2H), 3.35 (m, 1H), 6.58 (m, 1H), 6.81 (dd, 1H, 1.32 and 7.88 Hz), 7.08 (m, 2H), 7.23 (m, 3H), 7.34 (m, 3H), 7.47 (m, 2H), 7.62 (d, 1H, 7.92 Hz), 7.88 (d, 1H, 7.88 Hz), 7.99 (m, 2H). 13C NMR delta ppm: 8.33, 8.60, 21.46, 23.85, 27.66, 28.00, 28.57, 32.50, 32.90, 56.55 (10 sp3C), 118.89, 119.76, 120.75, 121.30, 121.49, 122.87, 124.27, 124.85, 125.30, 125.78, 126.22, 126.43, 127.18, 127.87, 128.23, 129.04, 130.86, 132.95, 134.91, 142.58, 142.88, 143.53, 145.02, 148.05, 148.19, 150.06, 151.86, 152.06, 154.29 and 169.02 (30 sp2C).

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, 1-Iodo-2-isopropylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; The United States of America, as represented by the Secretary of the Air Force; Tan, Loon-Seng; Kannan, Ramamurthi; (43 pag.)US10113065; (2018); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com