Month: September 2021

Related Products of 260355-20-2,Some common heterocyclic compound, 260355-20-2, name is 1-Chloro-4-iodo-2-(trifluoromethyl)benzene, molecular formula is C7H3ClF3I, 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.

1-Chloro-4-iodo-2-trifluoromethylbenzene (10 mmol) obtained in Reaction 1.2 was dissolved in 20 ml of toluene.Bis(pyridyl-2-methyl)amine (12 mmol) was added sequentially to the system.Palladium acetate (0.5 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (12 mmol), 3 ml of triethylamine,After stirring for 10 minutes, 10 ml of an aqueous solution of cesium carbonate (10 mmol) was added, and the mixture was heated to 50 C for 4 hours.After the reaction was completed, 20 ml of water was added to the system, stirred for 20 minutes, and liquid was separated.The organic phase is dried over anhydrous sodium sulfate, concentrated and purified by flash column chromatography.Yielding 3.3 g of yellow 4-chloro-N,N-bis(pyridinyl-2-methyl)-3-trifluoromethylaniline powder,The yield was 87.5%.

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

Reference:
Patent; Jingfan; Jing Fan; Ge Baoyin; Zhang Ruwei; Zhai Xuexu; (9 pag.)CN108633898; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, Name is 1,4-Diiodobutane, 628-21-7, 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.

5-Bromo-2- (4-methoxybenzyl) -7-methyliso-1-one at 0 C(3.0 grams, 8.7 moles)N, N-dimethylformamide (30mL)To the solution was added sodium hydride (1.043 g, 43.5 moles).The reaction solution was stirred at room temperature for 10 minutes.Then add 1,5-diiodopentane (3.493 g, 11.3 mol),The reaction solution was stirred at room temperature for 4 hours.After the reaction was monitored by TLC, the reaction was quenched with saturated ammonium chloride solution, and the mixture was extracted with ethyl acetate (100 mL x 2). The organic layers were combined, dried over anhydrous sodium sulfate, filtered and concentrated. The crude product was purified by flash column chromatography (petroleum ether / ethyl acetate = 1/1) to give the product in the form of an oil (1.97 hag, yield 56.8%).

Statistics shows that 1,4-Diiodobutane is playing an increasingly important role. we look forward to future research findings about 628-21-7.

Reference:
Patent; Nuowosida Pharmaceutical Co., Ltd.; Li Bing; (67 pag.)CN110256432; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 51560-21-5, These common heterocyclic compound, 51560-21-5, name is 1,4-Diiodo-2,5-dimethoxybenzene, 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.

Under nitrogen, the 7.8g 2,5-diiodo-1,4-methoxybenzene was dissolved in 50mL of dichloromethane, and at -78 condition, to the solution was added dropwise 5.58mL three boron bromide. After completion of the dropwise addition, stirred for 16 hours at room temperature, the solid was suction filtered to produce a large number, and dried in vacuo to give a white solid which is 2,5-diiodo-1,4-bis(hydroxy)benzene. Among these, 2,5-diiodo-1,4-di(methoxybenzene, boron tribromide in methylenechloride and the molar ratio of 1: 3:40;

The synthetic route of 51560-21-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shaanxi Normal University; Fang, Yu; Sun, xiaohuan; Cui, Hong; Qi, yanyu; Liu, ke; Wang, Gang; Chang, xingmao; (21 pag.)CN104031108; (2016); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 847685-01-2, 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. 847685-01-2, name is 4,5-Difluoro-2-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

16.1 (4-Chloro-phenyl)-(4,5-difluoro-2-iodo-phenyl)-diazene; Chloro-4-nitroso-benzene (9.1 g, 64 mmol; [932-98-9]) was added to a solution of 4,5-difluoro-2-iodo-phenylamine (10.9 g, 43 mmol; [847685-01-2]) in acetic acid (430 ml). The reaction mixture was heated under reflux conditions for 14 h. Ice water (1 1) and EtOAc (1 1) was added, the layers were separated and the aqueous layer was extracted two times with EtOAc. The combined extracts were washed with water and brine and dried over Na2SO4. The solvent was removed under reduced pressure and the residue was purified by column chromatography (silica gel, CH2Cl2/heptane) to give the title compound (4.34 g, 11 mmol; 27%) as orange solid. MS: m/e=377.9 [M+].

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, 4,5-Difluoro-2-iodoaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Benson, Gregory Martin; Bleicher, Konrad; Feng, Song; Grether, Uwe; Kuhn, Bernd; Martin, Rainer E.; Plancher, Jean-Marc; Richter, Hans; Rudolph, Markus; Taylor, Sven; US2010/76026; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 460-37-7, These common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, 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 479 mg (1.68 mmol) of the compound from Ex. 34A in 20 ml of DMF were added 582 mg (4.21 mmol) of potassium carbonate, and the mixture was stirred at RT for 15 min. Then 1.17 g (5.05 mmol) of 1,1,1-trifluoro-3-iodopropane were added, and the mixture was stirred at 50 C. for 20 h. The DMF was very substantially distilled off and the residue obtained was partitioned between semisaturated sodium chloride solution (100 ml) and ethyl acetate (50 ml). The water phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and concentrated. The residue obtained was chromatographed using a silica gel cartridge (Biotage, 100 g of silica gel, eluent: hexane/ethyl acetate 94:6?50:50). In this way, 517 mg (85% of theory) of the title compound were obtained. 1H-NMR (400 MHz, DMSO-d6, delta/ppm): 10.09 (s, 1H), 4.13 (d, 2H), 2.84-2.69 (m, 5H), 2.30-2.23 (m, 1H), 1.15 (d, 3H), 1.07-0.95 (m, 1H), 0.90-0.81 (m, 2H). LC/MS (Method 4, ESIpos): Rt=1.2 min, m/z=361 [M+H]+.

The synthetic route of 460-37-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bayer Aktiengesellschaft; Bayer Pharma Aktiengesellschaft; HAERTER, Michael; KOSEMUND, Dirk; CANCHO GRANDE, Yolanda; DELBECK, Martina; KALTHOF, Bernd; LUSTIG, Klemens; SUESSMEIER, Frank; US2020/16159; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 25245-27-6, name is 1-Iodo-3,5-dimethoxybenzene, 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 25245-27-6, Recommanded Product: 1-Iodo-3,5-dimethoxybenzene

1mmol of o-phenylenediamine, 1.2mmol of benzaldehyde, 1mmol3,5-dimethoxy iodobenzene as raw materials, into the 50mL pressure tube, using 10mol% CuSO4 as a catalyst, 2mmol KOH as a base,1,10-phenanthroline is used in an amount of 20 mol%N, N-dimethylformamide was used in an amount of 5 mL and the temperature was 120 C. The reaction was stirred for 24 h.The reaction solution was filtered through the residue and distilled under reduced pressure to give a white solid.The yield was 88% and 1- (3,5-dimethoxyphenyl) -2-phenyl-1H-benzimidazole was obtained as a white solid

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; Jiangsu Xian Ke Pharmaceutical Co., Ltd.; Liang Zhuowang; Huang Yuan; Xu Liangliang; (16 pag.)CN104557725; (2017); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 328-73-4, 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 328-73-4 as follows.

General procedure: In a round-bottomed flask filled with 50 mL of water, prop-2-ynyl-2-azidobenzoates (2a?b, 1.0 equiv), aryl halides (3a?j, 1.5 equiv), Pd(CH3CN)2Cl2 (2.5 mol percent), ligand 1b (5 mol percent) and iPr2EtN (3.0 equiv) were stirred vigorously under sonication at 80 °C for 30?40 min under atmospheric condition in the presence of CTAB (4 mmol). When TLC indicated completion of the reaction, the mixture was extracted with ethyl acetate (3 × 25 mL) and washed thoroughly with water. Column chromatography [silica gel (60?120), petroleum ether?ethyl acetate (5:1) as eluent] produced pure products (4a?j)

According to the analysis of related databases, 328-73-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Pal, Rammyani; Sarkar, Swarbhanu; Chatterjee, Nivedita; Sen, Asish Kumar; Tetrahedron Letters; vol. 55; 8; (2014); p. 1452 – 1455;,
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. 59528-27-7, name is (4-Iodophenyl)methanamine hydrochloride, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H9ClIN

Example 2 : Obtaining the 4-iodobenzylamide of 1- pentanoylamine-cyclopentanocarboxylic acid (VI) .8.2 g (18.6 mmol) of BOP is added to a suspension of 3.96 g (18.6 mmol) of 1-pentanoylamine-cyclopentanocarboxylic acid, 5.0 g (18.6 mmol) of hydrochloride of 4- iodobenzylamine and 6.5 mL (37,2 mmol) of diisopropylamine in 40 mL of dimethylformamide, and this is stirred for 10 hr . The reaction mixture is poured onto a mixture of EtOAc (400 mL) and water (400 mL) and stirred for 30 min. Following decanting, the organic phase is washed with saturated solution of sodium bicarbonate (200 mL x 2), with 5% solution of sodium bisulphite (200 mL) , with saturated solution of sodium chloride (100 mL) , dried with magnesium sulphate and evaporated. The residue is recrystallised from 60 mL of toluene to give 6.0 g (75%) of the title compound in the form of a white solid.M. p. = 150-152CIR (KBr, cm-1) : 3340, 3280, 1660, 1650, 1540.RMN IH (DMSO-d6), delta (ppm) : 0.80 (t, 3H, CH3) , 1.10-2.20(m, 14H), 4.20 (d, 2H, CH2-Ar) , 7.05 (d, 2H, H-Ar), 7.60(d, 2H. H.Ar) .

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 59528-27-7.

Reference:
Patent; INKE, S.A.; WO2006/89927; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 6828-35-9, 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 6828-35-9 as follows.

General procedure: A mixture of 2-iodoaniline 1 (0.5 mmol) and Pd(OAc)2 (5.6 mg, 0.025 mmol, 5.0 mol%) in CH3CN (3 mL) was added into a Schlenk flask (25 mL) and stirred at room temperature. Followed by the addition of ethyl acrylate 2a (100 mg, 1.0 mmol, 2.0 equiv) and triethylamine (101 mg, 1.0 mmol, 2.0 equiv), the mixture was stirred at 100 C until the reaction was finished. Then the mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate, 5:1 to 2:1) afforded the corresponding alkenylanilines 3.

According to the analysis of related databases, 6828-35-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Chen, Xia; Zhou, Xiao-Yu; Wang, Liang-Guang; Synthetic Communications; vol. 47; 22; (2017); p. 2096 – 2102;,
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. 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, A new synthetic method of this compound is introduced below., Product Details of 5876-51-7

The 248 mg (1mmol) 4 – bromophenylacetic methyl ether, 186 mg (2mmol) aniline, 9.5 mg (0.05mmol) CuI, 10.8 mg (0.05mmol) ligand L2, 424mg (4mmol) potassium phosphate, 1 ml ethanol,, adding 10 ml reaction tube, sealing, 25 C reaction under the condition 12h. After the stop of the reaction, water, extracted with ethyl acetate, washing, saturated salt water washing, after drying with anhydrous sodium sulfate, filtered, the filtrate is distilled under reduced pressure, purification by silica gel chromatography separation column column, shall be 3, 4 – methylenedioxy phenylaniline 192 mg, yield 90%.

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; Sun Yat-sen University; Wan Yiqian; Ding Xiaomei; Huang Manna; Zhu Xinhai; Yi Zhou; CN106883132; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com