Author: Jessica.F

Related Products of 111771-08-5, A common heterocyclic compound, 111771-08-5, name is 2-Fluoro-6-iodobenzoic acid, molecular formula is C7H4FIO2, 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.

W-Ethyl-2-fluoro-6-iodo-W-[(S)-1 -methyl-2-(5-trifluoromethyl-pyridin-2-yloxy)-ethyn (0350) (0351) D-1.1 (150 mg, 0.56 mmol) is dissolved in dry DCM (3.0 mL). Under stirring oxalylchloride (846 mg, 1 .13 mmol) and a drop of DMF are added and the mixture is stirred for 2 h. The mixture is concentrated and the residue is taken up with dry DCM (3.0 mL). The resulting mixture is added dropwise to a mixture of B-1 (145 mg, 0.51 mmol) and DIPEA (390 mu, 2.30 mmol) in DCM (4.0 mL) at 0C. The cold bath is removed and the mixture is stirred for 2 h. The crude product is diluted with DCM and washed with NH4CI (sat. solution), KHC03 (sat. solution) and water. The organic phase is dried and concentrated. The residue is purified by flash column chromatography (using a solvent gradient from 100% Cyclohexane to Cyclohexane/EA 65/35) to afford 160 mg of compound D-1. ESI-MS: 497 [M+H]+; HPLC (Rt): 1.21 min (Method P).

The synthetic route of 111771-08-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; RIETHER, Doris; FERRARA, Marco; HEINE, Niklas; LESSEL, Uta; NICHOLSON, Janet Rachel; PEKCEC, Anton; SCHEUERER, Stefan; (69 pag.)WO2017/178341; (2017); A1;,
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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 199786-58-8 as follows. Computed Properties of C7H6BrIO

A solution of oxalyl chloride (1.53 g, 0.012 mol) in CH2Cl2 (15 ML) was cooled to -70 C., and DMSO (1.41 g, 0.018 mol) in CH2Ck (15 ML) was added at -65 to -70 C. The mixture was stirred under nitrogen for 10 minutes at -70 C. and then treated with the product from Example 62B (2.35 g, 7.5 mmol) in 60 ML CH2Cl2.The slurry was stirred at -65 C. for 15 minutes and treated with triethylamine (3.8 g, 0.037 mol).The mixture was allowed to warm to -10 C. over 1 hour.The mixture was treated with 20 ML of water and allowed to warm to room temperature.The organic layer was separated and concentrated to provide the title compound. 1H NMR (CDCl3, 400 MHz) delta 9.97 (s, 1H), 7.97 (d, J=4 Hz, 1H), 7.79 (d, J=8 Hz, 1H), 7.40 (dd, J=4, 8 Hz, 1H). MS (DCl/NH3) [M+NH4]+ at 328.

According to the analysis of related databases, 199786-58-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Altenbach, Robert J.; Black, Lawrence A.; Chang, Sou-Jen; Cowart, Marlon D.; Faghih, Ramin; Gfesser, Gregory A.; Ku, Yi-yin; Liu, Huaqing; Lukin, Kirill A.; Nersesian, Diana L.; Pu, Yu-ming; Sharma, Padam N.; Bennani, Youssef L.; US2004/92521; (2004); A1;,
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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. 25245-35-6, name is 2-Iodo-1,4-dimethoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C8H9IO2

(3) Compound C (20.21 g, 98.0 mmol) was dissolved in benzene (150 mL), and 2,5-dimethoxyiodobenzene (27.16 g, 102.9 mmol), Pd (PPh3) was sequentially added at -15 C. 2Cl2 (0.69 g, 0.98 mmol), CuI (0.93 g, 4.9 mmol) and DIPEA (40 mL, 391 mmol),Then it was raised to 20 C to 30 C and stirred for 4 h.The reaction was quenched with EtOAc EtOAc (EtOAc)The combined organic layers were washed with brine (30 mL)After concentration under reduced pressure, the mixture was separated by column chromatography (hexane: ethyl acetate = 16:1).25.16 g of compound D was obtained in a yield of 75%(Rf = 0.38, n-hexane: ethyl acetate = 8:1).Among them, the detection data of compound D is as follows:

The synthetic route of 25245-35-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing University Shenzhen Sheng Yuan; Shao Wenbin; Huang Jun; Guo Kai; Zhang Weibin; Gong Jianxian; Yang Zhen; (47 pag.)CN108484638; (2018); A;,
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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. 101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C6H3ClFI

Preparation 9 IB: (2-Chloro-4-fluorophenyl)(3-fluoro-4-(pyrimidin-5-yl)pyridin-2- yl)methanoneTo a solution of 2-chloro-4-fluoro-l-iodobenzene (0.307 g, 1.199 mmol) in THF (Volume: 1.622 ml) cooled to -10 C was added isopropylmagnesium chloride, 2M in THF (0.699 ml, 1.399 mmol) in one portion. After 30 min, 3-fluoro-4-(pyrimidin-5- yl)picolinonitrile (0.200 g, 0.999 mmol) was added. The reaction mixture was stirred at -10 C for 30 min, then allowed to warm to room temperature and stirred overnight. Water and ice were carefully added, followed by acidification with 6 M HC1. After stirring for 1 hr, CH2C12 was added and the pH was adjusted to 8.5 with aqueous 4 M NaOH. The layers were separated. The aqueous phase was extracted with CH2CI2 (5X). Organics combined, dried over Na2S04, filtered, and concentrated to afford an orange residue. The crude material was dissolved in a minimal amount of CH2CI2 to be chromatographed. Purification of the crude material by silica gel chromatography using an ISCO machine (24 g column, 35 mL/min, 60-100% EtOAc in hexanes over 23 min, tr = 9 min) gave the title compound (0.029 g, 0.074 mmol, 7.44% yield) as an orange solid.

According to the analysis of related databases, 101335-11-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; BALOG, James Aaron; HUANG, Audris; VELAPARTHI, Upender; LIU, Peiying; WO2013/49263; (2013); A1;,
Iodide – Wikipedia,
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Related Products of 2265-91-0,Some common heterocyclic compound, 2265-91-0, name is 1,3-Difluoro-5-iodobenzene, molecular formula is C6H3F2I, 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.

10297] To a stirred solution of 5-(but-i-yn-i-yl)-i-(tetra- hydro-2H-pyran-2-yl)-1H-indazole (0.4 g, 1.574 mmol, Example 1, Step-3) in 2-methyl THF (5 mE), was added bis(pinacolato)diboron (0.44 g, 1.732 mmol), tetrakis(triphenylphosphine)platinum(0) (14.6 mg, 0.0118 mmol) under nitrogen atmosphere, reaction mixture was heated at 90 C. for 5 h. Afier completion of reaction (monitored by TEC), reaction mixture was allowed to cool to 4 C. and tert-butyl (2-(4-iodophenoxy)ethyl)carbamate (571 mg, 1.574 mmol, Example 3, Step-2), bis(triphenylphosphine)palladium(II) dichloride (55 mg, 0.078 mmol), cesium carbonate (1.023 g, 3.140 mmol) and 2-methyl THF (5 mE) were added. This mixture was degassed with nitrogen and water (1.2 mE) was added. Reaction mixture was stirred at room temperature for 16 h. Afier completion of reaction (monitored by TEC), i,3-difluoro-5-iodobenzene (528 mg, 2.20 mmol) and 4M aqueous KOH (3 mE) were added and the mixture was degassed with nitrogen and heated at 70 C. for 5 h. Upon completion, the reaction mixture was filtered through a celite/silicagel pad and washed with EtOAc. The filtrate was washed with water, brine, dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude product was purified by silica gel chromatography (2:8 EtOAc in n-hexane) to give title compound of Ex. 5 Step-i (500 mg, 54%)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3-Difluoro-5-iodobenzene, its application will become more common.

Reference:
Patent; Eisai R&D Management Co., Ltd.; BOCK, Mark; HAO, Ming-Hong; KORPAL, Manav; NYAVANANDI, Vijay Kumar; PUYANG, Xiaoling; SAMAJDAR, Susanta; SMITH, Peter Gerard; WANG, John; ZHENG, Guo Zhu; ZHU, Ping; (141 pag.)US2016/347717; (2016); A1;,
Iodide – Wikipedia,
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Application of 2142-70-3, These common heterocyclic compound, 2142-70-3, name is 1-(2-Iodophenyl)ethanone, 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.

[283] To a solution of 1-(2-iodophenyl)ethanone (4.0 g, 16.3 mmol) in a mixed solvent of chloroform (50 mL) and ethyl acetate (50 mL) was added cupric bromide (7.26 g, 32.5 mmol). The resulted mixture was stirred at reflux for 3h, then cooled down to roomtemperature, filtered, the filter cake was washed with ethyl acetate (50 mL), the filtrate was concentrated, the residue was purified by flash chromatography (petroleum ether: ethyl acetate= 50:1) to afford 2-bromo-1-(2-iodophenyl) ethanone (4.65 g, yield: 88%) as a light yellow oil.[284] ?H NIVIR (400 IVIFIz, CDC13-d): 7.98 (d, J = 8.0 Hz, 1H), 7.47 (d, J = 8.0 Hz, 2H), 7.19-7.21 (m, 1 H), 4.47 (s, 2H).

The synthetic route of 2142-70-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SHANGHAI DE NOVO PHARMATECH CO.,LTD.; LI, Qun; GAO, Daxin; (158 pag.)WO2016/131380; (2016); A1;,
Iodide – Wikipedia,
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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 351003-36-6 as follows. category: iodides-buliding-blocks

General procedure: A mixture of benzonitrile 1 (10.0 mmol) and methylhydrazine (2.8 mL, 50.0 mmol) in EtOH (10.0 mL) was heated to reflux overnight. The mixture was cooled to rt and then concentrated. H2O (10.0 mL) and EtOAc (20.0 mL) were added to the residue. The organic layer was washed with H2O (10.0 mL), brine (10.0 mL), dried over Na2SO4, filtered, and concentrated in vacuo. The residue was subjected to silica-gel chromatography by using EtOAc/hexanes (1:1) as eluent to give the product 2.

According to the analysis of related databases, 351003-36-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Han-Jun; Hung, Shiang-Fu; Chen, Chuan-Lin; Lin, Mei-Huey; Tetrahedron; vol. 69; 19; (2013); p. 3907 – 3912;,
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. 32024-15-0, name is 3-Iodo-4,5-dimethoxybenzaldehyde, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H9IO3

General procedure: To a solution of cycloalkenyl iodide (1.00 equiv) in Et 2 O (0.5 M) wasslowly added a solution of n-BuLi (2.44 M in hexane, 1.10 equiv) at-78 C. After stirring for 30 min at the aforementioned temperature, B(Oi-Pr)3 (1.15 equiv) and THF (total concn 0.25 M) were added andthe resulting mixture stirred for an additional 1 h at room tempera-ture. Pd(dppf)Cl2¡¤CH2C2 (4 mol%), the cross-coupling partner (aromatic or vinylic iodide, bromide, tosylate or chloride) (0.90 equiv) andan aqueous solution of NaOH (1.5 equiv 1.00 M) were subsequentlyadded and the reaction mixture was stirred overnight. The crude ma-terial was extracted with Et2O (3 ¡Á 20 mL), washed with a saturated aqueous solution of sodium chloride (20 mL), dried over magnesiumsulfate, filtered, concentrated and purified via flash column chroma-tography.

The synthetic route of 32024-15-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Baumann, Andreas N.; Eisold, Michael; Music, Arif; Didier, Dorian; Synthesis; vol. 50; 16; (2018); p. 3149 – 3160;,
Iodide – Wikipedia,
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Related Products of 628-21-7,Some common heterocyclic compound, 628-21-7, name is 1,4-Diiodobutane, molecular formula is C4H8I2, 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 50 mL flask compound 6 (100 mg, 0.43 mmol) and dry K2CO3 (80 mg, 0.50 mmol) were added to anhydrous DMF (3 mL). When the product was completelydissolved, an excess of 1,4-diiodobutane (0.5 mL) was added at room temperature. To the crude product distilled water (10 mL) was added and the solution was extracted three times with diethyl ether (30 mL). Then, the organic phase was washed three times with saturated aqueous NaCl solution(10 mL) and finally dried over Na2SO4. The product was purified by column chromatography(30%-60% CHCl3 in hexane), to give compound 7 was obtained as a white solid (237 mg, 0.39 mmol,91%).

The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Altieri, Alessandro; Alvino, Antonello; Ohnmacht, Stephan; Ortaggi, Giancarlo; Neidle, Stephen; Nocioni, Daniele; Franceschin, Marco; Bianco, Armandodoriano; Molecules; vol. 18; 11; (2013); p. 13446 – 13470;,
Iodide – Wikipedia,
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Electric Literature of 20555-91-3, These common heterocyclic compound, 20555-91-3, name is 1,2-Dichloro-4-iodobenzene, 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: The terminal alkyne (1.4 mmol), PdCl2 (5.0 mol%, 0.008 g), KOAc (3.0 mmol, 0.294 g), Cr(CO)6 (1.0 mmol, 0.22 g), hydroxylamine hydrochloride (1.5 mmol, 0.104 g), and aryliodide (1.0 mmol), DMF (3.0 mL) was added to a round-bottom flask. The reaction was heated at 70 C under air and stirred for 18h. The reaction mixture was washed with water and extracted with EtOAc (3¡Á10 mL). The solvent was evaporated and the product purified by flash column chromatography (n-hexane/EtOAc gradient: 0 to 20% EtOAc) to afford the corresponding isoxazole in high yield.

Statistics shows that 1,2-Dichloro-4-iodobenzene is playing an increasingly important role. we look forward to future research findings about 20555-91-3.

Reference:
Article; Iranpoor, Nasser; Firouzabadi, Habib; Etemadi-Davan, Elham; Tetrahedron Letters; vol. 57; 8; (2016); p. 837 – 840;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com