Month: March 2021

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
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. 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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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

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. 1219741-79-3, name is 4-Bromo-5-fluoro-2-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 4-Bromo-5-fluoro-2-iodoaniline

To a mixture of 4-bromo-5-fluoro-2-iodoaniline (step 1) (5.2 g, 16 mmol), Pd(PPh3)2Cl2 (582 mg, 0.83 mmol) and CuI (313 mg, 1.6 mmol) in 50 ml of Et3N was added ethynyltrimethylsilane (2.3 mL, 1.6 mmol) slowly at 0 C. The resulting mixture was degassed and charged with N2 three times. After stirring at 30 C. for 2 hrs, the reaction mixture was filtered over celite. The filtrate was diluted with ethyl acetate (*2), washed with water (*2) and brine (*2). The combined organic layers were dried over anhydrous Na2SO4 and filtered. The filtration was evaporated under reduced pressure to afford the crude product, which was purified by column chromatography on silica gel eluting with 0?5% ethyl acetate in hexanes to afford the title compound as yellow oil. LC-MS: Rt=1.29 mins; MS m/z [M+H]+ 286.0; Method 5-95AB 1.5minLC_v003 1H NMR (400 MHz, CDCl3) delta 7.19 (1H, d), 6.21 (1H, d), 4.11 (2H, s), 0.00 (9H, s).

The synthetic route of 1219741-79-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; CHEN, Shuhui; HE, Haiyang; LAGU, Bharat; QIN, Hua; WU, Chengde; XIAO, Yisong; US2015/183802; (2015); A1;,
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. 188815-32-9, name is 3-Bromo-5-iodobenzoic acid, A new synthetic method of this compound is introduced below., SDS of cas: 188815-32-9

Example 50 Synthesis of 3-Bromo-5-hydroxy-benzoic acid; The title compound was made according to the method described in Org. Proc. Res. Dev. 2002, 6, 591-595. To 5- iodo-3-bromo-benzoic acid (500 mg, 1.53 mmol), NaOH (250 mg, 6.1 mmol), Cu20 (240 mg, 1.68 mmol) was added water (4.0 mL). The mixture was heated for 1.5 h at 140 C in a sealed tube. The cooled mixture was diluted with water and extracted with CH2Cl2. The aqueous layer was acidified (pH-2) with TFA and extracted with EtOAc. The organic layer was dried over Na2S04, filtered, concentrated and purified by reverse-phase HPLC to yield 3-bromo-5-hydroxy-benzoic acid. ?H NMR (400 MHz, DMSO-d6): 10.30 (s, 1H), 7.46 (m, 1H), 7.31 (m, 1H), 7.17 (m, 1H).

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; AMGEN INC.; WO2005/113494; (2005); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 610-97-9, A common heterocyclic compound, 610-97-9, name is Methyl 2-iodobenzoate, molecular formula is C8H7IO2, 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.

2.27 g (15 mmol) was added sequentially to a 250 mL round bottom flask.Methyl 2-aminobenzoate, 3.93 g (15 mmol) of methyl 2-iodobenzoate,2.49 g (18 mmol) of potassium carbonate, 0.19 g (3 mmol) of activated copper powder and100mL of o-dichlorobenzene, degassing the reaction system, and then protecting with argon gas,The mixture was heated to 180 C with stirring and the reaction was continued for 48 h. After the reaction is complete,The system was cooled to room temperature, suction filtered under reduced pressure and the residue was washed with dichloromethane.After the filtrate was spin-dried, it was separated and purified on a silica gel column using an eluent of dichloromethane: petroleum ether = 3:1 (volume ratio).Obtained a yellow-green solid 3.66g,The yield was 85.6%.

The synthetic route of 610-97-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Soochow University (Suzhou); Liao Liangsheng; Yuan Yi; Jiang Zuoquan; (46 pag.)CN109456326; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com