Category: iodides-buliding-blocks

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. 21740-00-1, name is 5-Bromo-2-iodobenzoic acid, A new synthetic method of this compound is introduced below., Application In Synthesis of 5-Bromo-2-iodobenzoic acid

General procedure: The reaction of 2-iodobenzoic acid derivatives 1 and carbodiimides derivatives 2 is representative: A round bottom flask was added with 2-iodobenzoic acid derivatives 1 (0.50 mmol), carbodiimides derivatives 2 (1.0 mmol), Cu2O (0.25 mmol), in DMSO (2.5 mL). The reaction mixture was allowed to stir at 90 C for 18 hours. After completion of reaction, the reaction mixture was cooled to room temperature, quenched with 1M HCl, extracted with EtOAc, and DMSO was moved by distilled water. The combined organic layers were washed with brine and dried over anhydrous Na2SO4, filtered and concentrated. The residue was purified by column chromatography to provide quinazolinediones derivatives 3.

The synthetic route of 21740-00-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Duangjan, Chanikan; Rukachaisirikul, Vatcharin; Saithong, Saowanit; Kaeobamrung, Juthanat; Tetrahedron Letters; vol. 59; 39; (2018); p. 3537 – 3540;,
Iodide – Wikipedia,
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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. 914225-70-0, name is 1-(5-Fluoro-2-iodophenyl)ethanone, A new synthetic method of this compound is introduced below., Safety of 1-(5-Fluoro-2-iodophenyl)ethanone

Under a nitrogen atmosphere, a solution of compound 1 (2.6 g, 10 mmol) in methanol (50 mL) was cooled in an ice-water bath, into which NaBH4 (0.38 g, 10 mmol) was poured slowly, and continued to react at 0C for 5 minutes. 0.5M HCl solution was added dropwise slowly until no bubbles appeared in the reaction system. The reaction solution was adjusted to pH > 7 with saturated sodium bicarbonate solution, and extracted with ethyl acetate to obtain 2.6 g of a white solid product with a yield of 99%. LC-MS (APCI): m/z = 267 (M+1)+; 1H NMR (300 MHz, CDCl3)(delta/ppm)7.76-7.71 (m, 1H), 7.35-7.31 (m, 1H), 6.78-6.72 (m, 1H), 5.05-4.99 (m, 1H), 1.45 (d, J=6.0 Hz, 3H).

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; Shenzhen Targetrx, Inc.; WANG, Yihan; LI, Huanyin; (30 pag.)EP3415518; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 16355-92-3, 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. 16355-92-3, name is 1,10-Diiododecane, This compound has unique chemical properties. The synthetic route is as follows.

Measured into a 2-liter four-necked flask provided with a stirring device, a thermometer, and a reflux condenser were 197 g (0.5 mol) of 1,10-diiododecane, 520 g (4 mol) of ethyl acetoacetate, 1 L of ethanol, and 89.8 g (0.65 mol) of potassium carbonate, with reaction subsequently being allowed to take place for four hours under total reflux.After the reaction was completed, the ethanol, which was used as the solvent, was removed by distillation, and the remaining liquid was cooled to room temperature and subjected to liquid separation by adding 700 ml of 5% sulfuric acid. After the surplus of ethyl acetoacetate was removed by reduced pressure distillation of the organic layer at the upper layer. As a result, 237 g of an oily substance containing diethyl-2,13-bisacetyl-1,14-tetradecandioate was obtained.

The chemical industry reduces the impact on the environment during synthesis 1,10-Diiododecane. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Doya, Masaharu; US2011/172465; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 2043-57-4, 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 2043-57-4 as follows.

General procedure: 2-(Perfluorodecyl)ethyl iodide (5.26 g, 7.81 mmol), 4-mercaptophenol (0.94 g, 7.44 mmol), andK2CO3 (2.06 g, 14.88 mmol) was added in acetone (80 mL) in a 200 mL recovery flask, and theresulting mixture was heated at reflux for 3 days. The reaction mixture was allowed to cool toroom temperature. After 1 N HCl aqueous solution was added to the mixture until pH ? 3,saturated NaCl aqueous solution (100 mL) was added to it and the resulting solution wasextracted with EtOAc (100 mL × 3). The organic layers were combined and dried with MgSO4,and after filtration, the filtrate was concentrated using a rotary evaporator under reduced pressure.The crude product was purified by silica gel column chromatography (eluent: CHCl3) to give A-10 (3.00 g, 4.46 mmol) in 60% yield as colorless powder.

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:
Article; Yoshida, Tomohiro; Hirakawa, Tomomi; Nakamura, Toru; Yamada, Yasuhiro; Tatsuno, Hiroko; Hirai, Masayuki; Morita, Yuki; Okamoto, Hiroaki; Bulletin of the Chemical Society of Japan; vol. 88; 10; (2015); p. 1447 – 1452;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 124700-40-9, name is 2-Fluoro-4-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 124700-40-9, category: iodides-buliding-blocks

a. Methyl 2-fluoro-4-iodobenzoate (2). A modified procedure of Kakuta and co-workers was followed.2 2-Fluoro-4-iodobenzoic acid (5.35 g, 20.1 mmol) was dissolved in methanol (30 mL, 741 mmol) was added thionyl chloride (2.6 mL, 35.8 mmol), dropwise at 0 C with stirring. The reaction solution was then refluxed in an oil bath at 85 C for 1 hr. Excess methanol was removed in vacuo, and benzene (20 mL) was added to the residue and then removed in vacuo. To the residue was added ethyl acetate (150 mL), and the organic layer was washed with saturated NaHCO3 (200 mL) and brine (60 mL) and then dried over sodium sulfate, filtered and concentrated in vacuo. The crude product was purified by column chromatography (150 mL Si02, ethyl acetate:hexanes 1:48) to give 2 (5.3066 g, 94%) as a white crystalline solid, m.p. 76-78 C: 1H NMR (400 MHz, CDC13) 7.63 (t, J = 8.0, 1 H), 7.56 (dd, J= 8.4, 1.6, 1 H), 7.53 (dd, J = 10.0, 1.2, 1 H), 3.92 (s, 3H); ?3C NMR (100.6MHz, CDC13) 164.4, 164.3, 162.3, 159.7, 133.5, 133.4, 133.0, 126.5, 126.3, 118.2, 118.1, 99.8, 99.7, 52.5; JR (neat) n 2952, 1700, 1595, 1561 cm?; LC-FAB-MS (M)+ calcd for C8H6F102279.9397, found 279.9394.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Fluoro-4-iodobenzoic acid, and friends who are interested can also refer to it.

Reference:
Patent; ARIZONA BOARD OF REGENTS ON BEHALF OF ARIZONA STATE UNIVERSITY; WAGNER, Carl; MARSHALL, Pamela; JURUTKA, Peter; WO2015/130973; (2015); 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., Quality Control of 2-Iodo-4-methylaniline

General procedure: A mixture of 2-iodoaniline 1 (1 mmol), benzylamine 2 (1.2 mmol), sulfur powder (6 mmol), DABCO (2 mmol), Cu(OAc)2.H2O (0.02 mmol), and 1,10-phenanthroline (0.02 mmol) was stirredin DMSO (5 mL) at 100 C. After completion of the reaction as indicated by TLC, the mixture was cooled to room temperature, water (20 mL) was added, and then the aqueous solution was extracted with ethyl acetate (3 15 mL). The organic layers were combined, dried over anhydrous MgSO4, the filtrate was concentrated under vacuum and then the residue was purified by column chromatography (eluent: petroleum ether/ethyl acetate (10:1 to 14:1) on silicagel to provide the desired product.

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; Wang, Rui; Ding, Yong-Liang; Liu, Hong; Peng, Shu; Ren, Jie; Li, Lei; Tetrahedron Letters; vol. 55; 4; (2015); p. 945 – 949;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 351003-36-6, These common heterocyclic compound, 351003-36-6, name is 2-Fluoro-5-iodobenzonitrile, 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 2-fluoro-5-iodobenzonitrile (479.2 mg, 1 .94 mmol) in tetrahydrofuran (4 mL) at -20 C was added isopropylmagesium chloride (2 N, 0.97 ml, 1 .94 mmol) and the mixture was stirred for 1 hour. Then, a solution of the product of Example 1 b (200 mg, 1 .29 mmol) in tetrahydrofuran (0.5 mL) was added and the mixture was stirred at -20 C for an additional 1 hour, then warmed to room temperature and stirred for 1 hour. The reaction was quenched with saturated aqueous ammonium chloride (10 mL) and the organics were extracted with ethyl acetate (10 mL x 3). The combined phase was washed with brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: petroleum ether/ethyl acetate = 50:1 ) to afford the title compound as a white solid (200 mg, Yield: 48%). Mp = 1 17.9- 1 19.2 C; Rf = 0.2 (10:1 ) petroleum ether/: ethyl acetate); H NMR (400 MHz, CDCIs) delta 7.69-7.67 (m, 1 H), 7.64-7.60 (m, 1 H), 7.15 (d, J = 8.6 Hz, 1 H), 5.06 (d, J = 4.8 Hz, 1 H),1 .85 (d, J = 5.6 Hz, 1 H), 1 .83-1 .76 (m, 1 H), 1 .64- 1 .60 (m, 1 H), 1 .50-1 .44 (m, 3 H), 1 .32-1 .23 (m, 2 H), 1 .14 (s, 3 H), 1 .06 (s, 3 H), 1 .00-0.89 (m, 1 H), 0.53 (d, J = 6.4 Hz, 3 H) ppm; (ESI +ve) m/z 276 (M +H+); [a]D27 0 = +27.1 (c = 0.31 , dichloromethane).

The synthetic route of 351003-36-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIKAM PHARMACEUTICALS, INC.; GARVEY, David, S.; WO2012/174064; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 13421-00-6,Some common heterocyclic compound, 13421-00-6, name is 5-Chloro-2-iodobenzoic acid, molecular formula is C7H4ClIO2, 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 argon gas puged mixture of 2-iodo benzoic acids (1) (0.008 mol), Carbonyldiimidazole(0.008 mol) and K2CO3 (0.242 mol) in CH3CN (50 ml) was added Pd(OAc)2 (10 mol %) andstirred at 60 oC temperature for 12h. The reaction was monitored by TLC analysis. Aftercompletion of the reaction, the reaction mixture was poured carefully into ice-cold water (50mL) and the product was extracted with ethyl acetate (2 x 50 mL). The combined organic layerwas dried over anhydrous Na2SO4. After filtration, the solvent was evaporated under vacuum andthe crude product obtained was purified by column chromatography to afford the pure desiredproducts (2a-d).

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

Reference:
Article; Narsimha, Sirassu; Battula, Kumaraswamy; Vasudeva Reddy, Nagavelli; Synthetic Communications; vol. 47; 9; (2017); p. 928 – 933;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 181765-86-6, A common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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.

In a 500-mL round-bottom flask reactor, methyl 5-bromo-2-iodobenzoate (25.0 g, 73 mmol), 4-dibenzofuran boronic acid (18.7 g, 88 mmol), tetrakis (triphenylphosphine)palladium (1.7 g, 0.15 mmol), and potassium carbonate (20.2 g, 146.7 mmol) stirred together with toluene (125 mL), tetrahydrofuran (125 mL), and water (50 mL) for 10 hrs at 80 C. After completion of the reaction, the reaction mixture was cooled to room temperature and extracted with ethyl acetate. The organic layer thus formed was separated, concentrated in a vacuum, and purified by column chromatography to afford . (75.0 g, 60.1%).

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SFC CO., LTD.; Pyo, Sung-Wan; Shim, So Young; Lee, Yun-Ah; Yu, Se Jin; (129 pag.)US2017/133600; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 2142-70-3, name is 1-(2-Iodophenyl)ethanone, molecular formula is C8H7IO, 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: 1-(2-Iodophenyl)ethanone

To a cooled (-40 C) stirred solution of TiC4 (11 mL of a 1.0 M sol in DCM, 11 mmol) in 5 mL of DCM was added dimethyl zinc (5.5 mL of a 2 N sol. in toluene, 11 mmol). After stirring for 10 min iodoacetophenone (1.23 g, 5.0 mmol) was added. After 2 h the reaction was warmed to 0 C and stirred for an addtional 1 h. The reaction was poured onto ice and extracted with ether. The organic phase was washed with water and sat NaHCO3. The organic phase was dried over magnesium sulfate, filtered, and dried under reduced pressure. The material was distilled using a kugelrohr (80 C at 0.1 mm) to obtain 1.0 g (76% yield) of a clear oil ; H NMR (300 MHz, CDCI3) 8 7.71 (t, J = 2.0 Hz, 1 H), 7.51 (dt, J = 7.7, 1.3 Hz, 1 H), 7.35 (app d, J = 7.7 Hz, 1 H), 7.03 (t, J = 7. 9 Hz, 1 H), 1.29 (s, 9H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2142-70-3, its application will become more common.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; WO2005/87752; (2005); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com