Category: iodides-buliding-blocks

Synthetic Route 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.

500mL round-bottom flask reactor, methyl 5-bromo-2-iodo benzoate (25.0g, 73mmol) in 4-dibenzofuran boronic acid [0410] (18.7g, 88mmol), tetrakis (triphenylphosphine) palladium (1.7g, 0.15mmol), potassium carbonate (20.2 g, 146.7mmol) put the toluene 125 mL, tetrahydrofuran 125mL, water 50 mL. The temperature of the reactor was 80 C, 10 hours was stirred. When the reaction is complete cool down the temperature of the reactor to room temperature, extracted with ethyl acetate and the organic layer was separated It was. The organic layer was concentrated under reduced pressure and separated by column chromatography to give the intermediate 1-a. (75.0g, 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; PARK, SEOK BAE; SONG, JU MAN; LEE, YUR IM; KIM, HEE DAE; PARK, SANG WOO; JEONG, KYUNG SEOK; CHA, SOON WOOK; (96 pag.)KR2015/130206; (2015); A;,
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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 573764-31-5 as follows. Recommanded Product: 573764-31-5

3) Preparation of 4-chloro-3-(4,4,5,5,-tetramethyl-1,3,2-dioxaborolan-2-yl)aniline (compound 1-5) A mixture of compound 1-4 (10 g, 39.5 mmol), 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi(1,3,2-dioxaborolane) (20.0 g, 79.0 mmol), KOAc (11.6 g, 118.5 mmol), and PdCl2(dppf) (960 mg, 1 mmol) in 1,4-dioxane (60 mL) was stirred at 105¡ã C. for 8 h under N2. The reaction mixture was concentrated in vacuo, and the residue was purified by column chromatography (hexanes/dichloromethane: 3/1 to 1/1) to afford compound 1-5 as a light yellow solid (6.0 g, 60percent yield). LCMS: m/z 295.1 [M+42]+. 1H NMR (400 MHz, CDCl3): delta 1.36 (s, 12H), 3.61 (br, 2H), 6.65 (dd, J=8.8 Hz, 2.8 Hz, 1H), 7.00 (d, J=2.8 Hz, 1H), 7.11 (d, J=8.8 Hz, 1H).

According to the analysis of related databases, 573764-31-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Genetech, Inc.; Curis, Inc.; Cai, Xiong; Qian, Changgeng; Zhai, Haixiao; US2014/18368; (2014); A1;,
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Synthetic Route of 74534-15-9, 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. 74534-15-9, name is 1-Chloro-2-iodo-4-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The appropriate product 2 (1 mmol, 1 eq) in AcOH/EtOH (1:1, 0.42 M) was added slowly to a solution of Iron powder (6 eq) in AcOH/EtOH(1:2, 2 M) at 60C . The solution was stirred at 70C for 30-60 mins. The reaction mixture was cooled to 23C , filtered through celite, washed with ethyl acetate, and concentrated. The oily residue was dissolved in ethyl acetate (30 mL), washed with saturated aq. NaHCO3 (1 x 15 mL), water (2 x 10 mL), dried (MgSO4) and concentrated. The oily residue was used without further purification.

The synthetic route of 1-Chloro-2-iodo-4-nitrobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Fangying; Jiang, Hongxia; Deng, Yufang; Yu, Jiang; Zhan, Miao; Zhao, Lifeng; Chen, Yuanwei; Bioorganic and Medicinal Chemistry Letters; vol. 28; 14; (2018); p. 2399 – 2402;,
Iodide – Wikipedia,
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These common heterocyclic compound, 74534-15-9, name is 1-Chloro-2-iodo-4-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. HPLC of Formula: C6H3ClINO2

The appropriate product 2 (1 mmol, 1 eq) in AcOH/EtOH (1:1, 0.42 M) was added slowly to a solution of Iron powder (6 eq) in AcOH/EtOH(1:2, 2 M) at 60C . The solution was stirred at 70C for 30-60 mins. The reaction mixture was cooled to 23C , filtered through celite, washed with ethyl acetate, and concentrated. The oily residue was dissolved in ethyl acetate (30 mL), washed with saturated aq. NaHCO3 (1 x 15 mL), water (2 x 10 mL), dried (MgSO4) and concentrated. The oily residue was used without further purification.

The synthetic route of 1-Chloro-2-iodo-4-nitrobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Fangying; Jiang, Hongxia; Deng, Yufang; Yu, Jiang; Zhan, Miao; Zhao, Lifeng; Chen, Yuanwei; Bioorganic and Medicinal Chemistry Letters; vol. 28; 14; (2018); p. 2399 – 2402;,
Iodide – Wikipedia,
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Electric Literature of 355-43-1, These common heterocyclic compound, 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, 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: A 25 mL of Schlenk tube equipped with a magnetic stir bar were charged with aniline (1.2 mmol, 3.0 equiv), K2CO3 (0.8 mmol, 2.0 equiv) and fac-Ir(ppy)3 (0.26 mg, 0.0004 mmol, 0.1 mol %) under air. The vessel was evacuated and backfilled with Ar (3 times), CnF2n+1I (n=6, 4, 2; 0.4 mmol, 1.0 equiv), anhydrous 1,2-dichloroethane (4 mL) were then added. The tube was screw capped and stirred at room temperature under irradiation of blue LEDs (12 W) for 24 hours. The reaction mixture was filtered through a pad of Celite and washed with ethyl acetate (3¡Á5 mL). The filtrate was concentrated. The residue was subjected to column chromatography on silica gel to afford the pure product.

The synthetic route of 355-43-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; He, Chun-Yang; Gu, Ji-Wei; Zhang, Xingang; Tetrahedron Letters; vol. 58; 41; (2017); p. 3939 – 3941;,
Iodide – Wikipedia,
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619-58-9, name is 4-Iodobenzoic acid, 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

248 mg (1 mmol) of 4-iodobenzoic acid and 720.54 mg (3 mmol) of sodium sulfide nonahydrate were added, copper powder 12.70 mg (0.2 mmol), ethanedithiol 8.4 uL (0.1 mmol) and 3 mL of solvent DMSO was placed in a 25 mL reaction tube equipped with a magnet, sealed with argon, heated and stirred, and reacted in an oil bath at 90 C for 12 hours. After completion of the reaction, the reaction solution was washed with NaOH solution and transferred to a 250 mL separatory funnel. The ether was extracted and the upper organic solvent was removed. The aqueous phase was adjusted to pH 1-3, extracted with dichloromethane and washed with water. Dried over magnesium sulfate. Evaporated under reduced pressure and subjected to column chromatography to afford 152 mg of product as a white solid, yield 99%

The synthetic route of 619-58-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dalian University of Technology; Liu Yajun; Xue Hongyu; Jing Bing; Liu Yong; (18 pag.)CN106916090; (2017); A;,
Iodide – Wikipedia,
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Application of 1131614-23-7, 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. 1131614-23-7, name is Methyl 4-(difluoromethoxy)-3-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of methyl 4-(difluoromethoxy)-3-iodobenzoate (2 g, 6.1 mmol) from step 1 , 2-ethynylpyridine (0.94 ml_, 9.2 mmol), dichlorobistriphenylphosphine palladium(ll) (0.86 g, 1.2 mmol), copper iodide (0.23 g, 1.2 mmol) and triethylamine(1.7 ml_, 12.2 mmol) in toluene (30 ml.) was stirred at 100 0C under an atmosphere of nitrogen for six hours. After the reaction was complete, the reaction mixture was concentrated to yield a semi-solid residue. This residue was purified by flash chromatography on SiO2 (gradient elution using EtOAc/hexane 20/80) to yield the title compound as a white solid (1.47 g, 80% yield).

The chemical industry reduces the impact on the environment during synthesis Methyl 4-(difluoromethoxy)-3-iodobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; WYETH; WO2009/143404; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 51628-12-7, name is 2-(4-Iodophenyl)acetonitrile, 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 51628-12-7, Recommanded Product: 2-(4-Iodophenyl)acetonitrile

(1) A three-necked flask was added with p-iodobenzeneacetonitrile (0.04 mol), phloroglucinol (0.02 mol) and etherAgent, zinc chloride (0.012 mol) as a catalyst, HCl gas (30 ml) was bubbled in an ice-salt bath for 1 hour to observe the reactionThe medium should change from colorless to orange. The reaction was allowed to stand in the freezer for 12 hours, and then continued to pass HCl gas (25ml)1 hour, standing in the refrigerator for 2 days, remove the reaction solution, decanting ether, water bath heated to reflux for two hours, was recrystallizedTo 2,4,6-trihydroxy-4′-iodo-phenylbenzyl ketone of general formula IIa.

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Reference:
Patent; Nanhua University; Zheng Xing; Zheng Qutong; Wang Zongbao; Lei Xiaoyong; Zeng Xianliang; Xiao Yan; Liu Ya; Huang Qiuxia; (23 pag.)CN106432165; (2017); A;,
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. 6940-76-7, name is 1-Chloro-3-iodopropane, A new synthetic method of this compound is introduced below., Formula: C3H6ClI

To a suspension of NaH (22 mg, 0.85 mmol) in DMF (2.0 mL) was added S1 (305 mg, 0.78 mmol) in DMF (1.5 mL). After 10 min at room temperature, S4a (0.20 mL, 1.53 mmol) was added to this mixture, and the reaction mixture was stirred at room temperature for 6 h, diluted with ether,washed with water and dried over Na2SO4. Purification by FCC (PE/EtOAc, 8 : 1) gave the chloride S5a (344 mg, 94%) as a yellow oil.

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; Gao, Yan; Shan, Dong; Jia, Yanxing; Tetrahedron; vol. 70; 34; (2014); p. 5136 – 5141;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, 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. Application In Synthesis of 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane

General procedure: In a three-necked round flask, 9-decene-1-ol (5.0mmol) and perfluoroalkyl iodide (6.0mmol) were dissolved in a mixture of CH3CN and H2O (1:1, 10mL total). Sodium dithionate (Na2S2O4) (5.8mmol) and sodium hydrogen carbonate (NaHCO3) (5.2mmol) were added to the reaction mixture and the solution was stirred at room temperature for 4h. The reaction mixture was extracted with ethyl acetate and washed three times with water. The organic layer was dried over sodium sulfate (Na2SO4), filtered, and evaporated to yield 3a (2.433g, 96.9%) or 3b (2.786g, 92.6%) as yellow liquid.

The synthetic route of 355-43-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Miyajima, Hiroki; Kasuya, Maria Carmelita Z.; Hatanaka, Kenichi; Journal of Fluorine Chemistry; vol. 222-223; (2019); p. 24 – 30;,
Iodide – Wikipedia,
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