Tag: M.W=200-300

Related Products of 4387-36-4,Some common heterocyclic compound, 4387-36-4, name is 2-Iodobenzonitrile, molecular formula is C7H4IN, 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.

Weigh 2.28 g of o-iodobenzonitrile and 1.13 g of phenylacetylene. Bis-triphenylphosphine palladium dichloride 140mg, 19 mg of cuprous iodide is dissolved in 250 mL of triethylamine. The reaction was carried out under nitrogen at 60 C for 12 h. Thin chromatography was used to detect the reaction process. After the reaction is completed, it is filtered with diatomaceous earth. Rotating off the solvent triethylamine, dry loading by column chromatography to obtain a pale yellow solid 1.86 g (yield 91%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Iodobenzonitrile, its application will become more common.

Reference:
Patent; Zhengzhou University; Chen Xiaolan; Sun Kai; Yu Bing; Qu Lingbo; Sun Yuanqiang; (8 pag.)CN108689892; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 16932-44-8, name is 2-Iodo-1,3-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 16932-44-8, name: 2-Iodo-1,3-dimethoxybenzene

General procedure: A 2.64 M solution of n-BuLi in hexane (0.4 mL, 1.0 mmol) was added dropwise to a solution of 4 (200 mg, 0.69 mmol) in DME (2 mL) at 0 C under Ar. The mixture was stirred at room temperature for 30 min, before CuCl (109 mg, 1.11 mmol) was added in one portion. Stirring was continued at room temperature for 1 h, before pyridine (0.53 mL, 6.4 mmol) and 3-iodoanisole (234 mg, 1.00 mmol) were added in one portion. Subsequently, the mixture was heated to 100 C for 45 h. After cooling, the reaction was quenched with 10% aq. HCl, before the insoluble materials were removed by filtration through Celite. The filtrate was extracted with AcOEt, and the organic fractions were washed with 10% aq. Na2S2O3 and brine, dried over Na2SO4, and concentrated. Purification by column chromatography on silica gel (eluent: n-hexane) afforded a mixture of 5 and unreacted 3-iodoanisole. A 1 M solution of TBAF in THF (0.79 mL, 0.79 mmol) was added to the mixture in 2 mL of dry THF, before the reaction mixture was stirred for 4 h at room temperature. The reaction was quenched with water and the reaction mixture was extracted with AcOEt. The organic layer was washed with brine, dried over Na2SO4, and concentrated. Purification by column chromatography on silica gel (eluent: n-hexane to n-hexane/AcOEt = 10/1, v/v) afforded 2b as a colorless solid in 67% yields over two steps.

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; Kaise, Asako; Ohta, Kiminori; Endo, Yasuyuki; European Journal of Medicinal Chemistry; vol. 122; (2016); p. 257 – 263;,
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. 60577-34-6, name is 4-Iodo-N-methylaniline, A new synthetic method of this compound is introduced below., Safety of 4-Iodo-N-methylaniline

(4) 7.7 g (33 mmol) of 4-iodo-N-methylaniline, 3.9 g (38 mmol) of acetic anhydride and 3.0 g (38 mmol) of pyridine,After reacting at room temperature for 1 hour, 50 ml of water was added to the reaction mixture, and the product was extracted with chloroform.After the reaction, usual post-treatment was performed to obtain 8.6 g of a yellow solid.This yellow solid was recrystallized using a mixed solvent of diethyl ether: ethanol = 5: 1 (v / v),7.6 g (84% yield) of 4-iodo-N-methylacetanilide was obtained as a yellow solid.

The synthetic route of 60577-34-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Unimatec Co., Ltd.; Saito, Satoshi; (9 pag.)JP5895454; (2016); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 5876-51-7, 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 5876-51-7 as follows.

[00411] In a reaction tube under nitrogen, a mixture of PdCl2(dppf)CH2Cl2 (24 mg; 0.029 mmol) and triethylamine (0.36 ml; 2.58 mmol) in dimethylsulphoxide (4 ml; dried over 4 A sieves) was sealed and stirred at 80 C. for 18 hours. After cooling to room temperature HB(pin) (0.19 ml; 1.31 mmol) was added followed by 1-iodo-3,4-methylenedioxybenzene (211. mg; 0.851 mmol). The reaction mixture was stirred at 80 C. GC analysis after 18 hours showed that the desired arylborate compound had formed.

According to the analysis of related databases, 5876-51-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Commonwealth Scientific and Industrial Research Organisation; US6680401; (2004); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 77317-55-6, 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. 77317-55-6, name is Methyl 2-amino-5-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 3, Preparation of Methyl 2-(acetoacetylamino)-5-iodobenzoate.; A solution of methyl 2-amino-5-iodobenzoate (17.9 g, 64.6 mmol) and methylacetoacetate (7.0 mL, 64.6 mmol) in toluene (250 mL) was heated to reflux using a Soxhlet extractor filled with 3 angstrom molecular sieves. After 24 h, the molecular sieves were replaced, more methylacetoacetate (3.75 mL, 32.3 mmol) was added, and the solution was refluxed 2 days. Concentration in vacuo and wash with diethyl ether afforded 24.7 g (76%) of methyl 2-(acetoacetylamino)-5-iodobenzoate as an off-white powder. LCMS: Rt = 1.70 min, [MH+362.0].

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, Methyl 2-amino-5-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MILLENNIUM PHARMACEUTICALS, INC.; WO2005/118583; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 29289-13-2, 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. 29289-13-2, name is 2-Iodo-4-methylaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

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.

The synthetic route of 2-Iodo-4-methylaniline has been constantly updated, and we look forward to future research findings.

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. 612-55-5, name is 2-Iodonaphthalene, A new synthetic method of this compound is introduced below., Recommanded Product: 612-55-5

General procedure: All reactions were carried out in an 80 mL Teflon-lined stainless steel reactor equipped with a magnetic stirring bar. Typically, in a glovebox, the aryl iodides (1.0 mmol), RhI3(0.025 mmol), PPh3 (0.1 mmol), Et3N (1.2 mmol), and DMA (2 mL) were loaded into the reactor. Then, the autoclave was screwed up, charged with CO and H2 to a total pressure of 10 bar (1:1) and transferred to an oil bath preheated at 90 C, which was controlled by a Haake-D3 temperature controller. After completion of the reaction, the reactor was cooled in iced water and the gas carefully vented. The conversion and yield of the aryl iodides and arylaldehydes were determined by GC analysis using dodecane as an internal standard. For yield determination of the other products, the reaction mixture was first analyzed by GC-MS to determine the structures of the aromatic aldehyde products. Then, CH2Cl2 (5 mL) was added to the reaction mixture, after which deionized water (10 mL) was added to extract the solvent DMA for 5 times. The organic layer was dried over anhydrous Na2SO4, concentrated by rotary evaporation and finally purified by column chromatography on silica gel using n-hexane/ethyl acetate as eluent to obtain the pure products and isolated yields.

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; Chen, Suqing; Liu, Zhenghui; Mu, Tiancheng; Wang, Peng; Yan, Zhenzhong; Yu, Dongkun; Zhao, Xinhui; Beilstein Journal of Organic Chemistry; vol. 16; (2020); p. 645 – 656;,
Iodide – Wikipedia,
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Electric Literature of 103962-05-6, 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. 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

in room temperature,4-Trifluoromethoxyiodobenzene (1.2 mmol, 3 equiv),Elemental selenium (1.2 mmol, 3 equiv),5-phenyl-1,3,4-oxadiazole (0.4 mmol, 1 equiv),Cu (OAc) 2 (0.04 mmol),Potassium carbonate (1.2 mmol, 3 equiv) was added to the reaction tube,Then filled with nitrogen, and replaced three times, in the nitrogen reaction environment,Then, 2 mL of DMF was added to the reaction solvent and stirred at 140 ¡ã C for 24 h.After the reaction was monitored by thin layer chromatography, the reaction mixture was cooled,Then diluted with ethyl acetate, and the diluted solution was transferred to a separatory funnel,Extracted with saturated brine, separated from the aqueous phase and organic phase, and then extracted with ethyl acetate 3 times,The organic phases were combined, 5 g of anhydrous sodium sulfate was added,Wash the filter cake with 5 mL of ethyl acetate each time 3 times, then spin off the solvent,The product was isolated by column chromatography (eluent: petroleum ether: ether = 98: 2)The product was a yellow solid in 57percent yield and 88 mg of product.

The synthetic route of 1-Iodo-4-(trifluoromethoxy)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wenzhou Medical University; Wu Ge; (23 pag.)CN107056727; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 25309-64-2, name is 1-Ethyl-4-iodobenzene, 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 25309-64-2, Quality Control of 1-Ethyl-4-iodobenzene

General procedure: After standard evacuation and back-fill cycles with argon, a Schlenk tube fitted with a magnetic stirrer bar was charged with pyrazole derivative (1.29 mmol), aryl iodide (1.1 eq), K3PO4 (2 eq) and copper iodide (0.1 eq). N,N’-dimethyl-cyclohexane-1,2-diamine (0.2 eq) and anhydrous dioxane (3 mL) were then added under a stream of argon by syringe at room temperature. The sealed tube is stirred at 110 C for 24-48 h. A 28% solution of ammonia and water are added at room temperature to the reaction mixture. The resulting aqueous layer is extracted with DCM. The combined organic layers are dried on MgSO4, filtered and evaporated under reduced pressure. The residue is triturated in an appropriate solvent or purified on silica gel.

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; Deprez-Poulain, Rebecca; Cousaert, Nicolas; Toto, Patrick; Willand, Nicolas; Deprez, Benoit; European Journal of Medicinal Chemistry; vol. 46; 9; (2011); p. 3867 – 3876;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 2265-91-0, 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 2265-91-0 as follows.

A mixture of compound 1 (15mg, 0.085mmol), compound 2(24mg, 0.1mmol), CS2CO3 (110mg, 0.34mmol), Pd(dba)2(5mg, 0.0085mmol) and Xanphos (4mg, 0.0085mol) in DMF(1.0mL) were degassed under N2 and then heated to 100 C for lh. After cooled, the reaction mixture was filtered. The filtrate was washed with H2O, extracted with EtOAc. The organic layer was dried over anhydrous Na2S04, filtered and concentrated to residue, which was purified by prep-TLC (EA/PE, 1/2, v/v) to give desired compound (6mg, 25% yield). LCMS: m/z, 303.0(M+H)+; 1H NMR (400MHz, CDCl3): delta 2.47~2.73(m, 2H), 3.49~3.55(m, 2H), 3.78(s, 1H), 3.85(s, 1H), 6.02~6.06(m, 2H), 6.15~6.19(m, 1H), 7.30~7.34(m, 1H), 7.51(d, J=8.0Hz, 1H), 7.69~7.73(m, 1H), 8.63(d, J=4.4Hz, 1H).

According to the analysis of related databases, 2265-91-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HUA MEDICINE (SHANGHAI) LTD.; CHEN, Li; BALDWIN, John J.; WU, Chengde; SHEN, Chunli; WO2014/124560; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com