Category: iodides-buliding-blocks

Synthetic Route of 450412-28-9, 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. 450412-28-9, name is 1-Bromo-3-chloro-2-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Intermediate A1 (95.2 g, 0.29 mol),1-Bromo-3-chloro-2-iodobenzene (109.1 g, 0.34 mol),Copper Iododide (54.5 g, 0.29 mol) and K3PO4 (182.1 g, 0.86 mol) were placed in dimethylacetamide (950 mL) and the mixture was refluxed and stirred.After the reaction was completed, the reaction solution was cooled to room temperature and then copper was removed by filtration. The solution in which the product was dissolved was reduced in pressure to remove all of the solvent. Then, the solution was completely dissolved in CHCl 3 and washed with water. The solvent was then removed under reduced pressure, and the resulting product was purified by column chromatography to obtain 132.1 g of intermediate A2 (yield: 88% .

The synthetic route of 1-Bromo-3-chloro-2-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LG Chem, Ltd.; Lee Jeong-ha; Park Tae-yun; Lee Dong-hun; Kim Min-jun; (39 pag.)KR2018/40100; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 75581-11-2, 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. 75581-11-2, name is 4-Iodo-1-methoxy-2-methylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

[00359] In a reaction tube under nitrogen, a mixture of PdCl2(dppf)CH2Cl2 (21 mg; 0.026 mmol) and triethylamine (0.34 ml; 2.44 mmol) in dioxane (2.5 ml; dried over 4 A sieves) was sealed and stirred at 80 C. overnight (18 h). After cooling to room temperature, HB(pin) (0.19 ml; 1.31 mmol) was added followed by 1-iodo-4-methoxy-3-methylbenzene (215 mg; 0.867 mmol) in dioxane (2.5 ml; dried over 4 A sieves) and the reaction mixture was stirred at 80 C. GC analysis after 18 hours showed a single new peak at 11.4 minutes which was identified by GC/MS as the desired arylborate compound.

The synthetic route of 4-Iodo-1-methoxy-2-methylbenzene has been constantly updated, and we look forward to future research findings.

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

Application of 3819-88-3,Some common heterocyclic compound, 3819-88-3, name is 1-Fluoro-3-iodo-5-nitrobenzene, molecular formula is C6H3FINO2, 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 1.0 eq IA in dry DMF (0.37 M) was added Zn(CN)2 (0.92 eq) and Pd(PPli3)4 (0.058 eq). The reaction mixture was purged with nitrogen and heated to 800C overnight. An additional 0.023 eq of Pd(PPh3)4 was then added and the reaction was heated for another 6 hrs. The reaction mixture was then cooled to RT, diluted with 15 volumes of EtOAc (based on IA) and the organic layer was washed 3 times with water and once with brine. The organic layer was dried over sodium sulfate, filtered and concentrated. Purification by chromatography over silica gel using 10% Et2O/hexane as the eluant provided IB as a solid (90%).

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

Reference:
Patent; CYTOKINETICS, INC.; WO2007/70626; (2007); A2;,
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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 4-Bromo-1-iodo-2-nitrobenzene

(1) In the reaction flask, add naphthobenzofuran-6-boronic acid (100mmol), 2-iodo-5-bromonitrobenzene (100mmol), 0.9g (0.785mmol, 0.5%) tetratriphenylphosphine palladium , 500mL of toluene, 200mL of ethanol, 200mL of water and 40g (300mmol) of potassium carbonate, react at 100 C for 8h; after the reaction is complete, stop the reaction; cool to room temperature, separate the organic phase, concentrate, silica gel column chromatography to obtain yellow powder M1;

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; Yantai Xianhua Chemical Technology Co., Ltd.; Xing Qifeng; Feng Peichuan; Chen Yue; Hu Lingfeng; Chen Yili; (24 pag.)CN110734446; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 188815-32-9,Some common heterocyclic compound, 188815-32-9, name is 3-Bromo-5-iodobenzoic acid, molecular formula is C7H4BrIO2, 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.

INTERMEDIATE 9; 2′-Fluoro-5-formyl-N-isopropyl-4′-methylbiphenyl-3-carboxamide; Step A: Methyl 3-bromo-5-iodo-benzoate; Methanol (50 mL) was added into a solution of 3-bromo-5-iodo-benzoic acid (25 g) in 2MHCl/ether (100 mL). The reaction mixture was then stirred at room temperature for 18 hrs. The solution was dried down under reduced pressure. The residue was then re-dissolved in ethyl ether (300 mL). The ether solution was washed with sat. Na2CO3 (3×200 mL), and water (3×200 mL). The organic layer was dried with sodium sulfate and evaporated to dryness to give the crude product. The crude product was then purified through a short silica column (eluted with 20% EtOAc/hexane) to give pure compound by TLC.

The synthetic route of 188815-32-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK & CO., INC.; WO2009/58298; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 51628-12-7, 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. 51628-12-7, name is 2-(4-Iodophenyl)acetonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 94 Synthesis of N-{2-[4-(3-(3-pyridyl)-4-methoxyphenyl)aminophenyl]ethyl}-(R)-2-hydroxy-2-(8-hydroxy-2(1H)-quinolinon-5-yl)ethylamine (94) Compound 94: Formula (XI) where R11 is 3-pyridyl a.Synthesis of 4-iodophenethylamine 4-Iodophenylacetonitrile (4.80 g, 19.7 mmol) was dissolved in tetrahydrofuran (25 ML) under nitrogen, and 1.0 M borane in tetrahydrofuran (29.6 ML, 29.6 mmol) was added via syringe.The reaction was heated at reflux for 1 hour, then cooled in ice and the excess borane was quenched by the addition of methanol (100 ML).When hydrogen evolution ceased, the solvents were removed under reduced pressure.The residue was dissolved in tetrahydrofuran (25 ML) and 4N HCl in dioxane (6.0 ML, 24 mmol) was added, followed by ether (75 ML).The hydrochloride salt of 4-iodophenethylamine was collected on a Buchner funnel, washed with ether (2*50 ML) and dried under reduced pressure.To generate the free base, the solid was partitioned between dichloromethane (200 ML) and 1N NaOH (100 ML).The aqueous layer was extracted with dichloromethane (2*100 ML).The combined organic layers were dried (Na2SO4) and concentrated to give 4-iodophenethylamine (4.52 g) as a colorless oil.

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, 2-(4-Iodophenyl)acetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Moran, Edmund J.; Jacobsen, John R.; Leadbetter, Michael R.; Nodwell, Matthew B.; Trapp, Sean G.; Aggen, James; Church, Timothy J.; US2003/229058; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 19094-48-5, name is 3,5-Diiodobenzoic acid, molecular formula is C7H4I2O2, 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. SDS of cas: 19094-48-5

Step 2: Methyl 3,5-diiodobenzoate (YZ-I-93) To a solution of 3,5-diiodobenzoic acid (6.8 g, 18.18 mmol) in methanol (200.0 ml) was added CH3SO3H (0.5 ml). The reaction mixture was heated to reflux. After refluxing for 7.5 hours, most of the methanol was removed. Then, water (200.0 ml) was added and a dark-brown solid was collected by filtration. The product was purified by silica gel column chromatography using hexanes/ethyl acetate (8:2) as eluent. The final pure white product was obtained in the amount of 4.2 g (59.2%) by recrystallization from methanol/water: 1H NMR (CDCl3): delta 8.29 (d, 2HBz, J=1.6 Hz), 8.20 (t, 1HBz, J=1.6 Hz), 3.90 (s, 3H, OCH3). 13C NMR (CDCl3): delta 163.97, 148.99, 137.56, 133.08, 94.32, 52.73.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 19094-48-5, its application will become more common.

Reference:
Patent; GEORGIA TECH RESEARCH CORPORATION; US2010/331509; (2010); 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 13194-68-8 as follows. Computed Properties of C7H8IN

To a solution of 4-iodo-2-methylaniline (4.0 g, 17 mmol) and Pd(dppf Cl2 (140 mg, 0.17 mmol) in THF (50 mL) was added isopropylmagnisium chloride (25.5 mL, 51.0 mmol) at -78 C and was reacted at reflux for 4 h. The reaction was quenched with a saturated solution of NH4C1, extracted with EtOAc, dried over anhydrous Na2SC>4, filtered, and concentrated to dryness. The residue was purified by flash column chromatography to give the title Compound as a brown solid (320 mg).

According to the analysis of related databases, 13194-68-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; ARORA, Nidhi; BACANI, Genesis M.; BARBAY, Joseph Kent; BEMBENEK, Scott D.; CAI, Min; CHEN, Wei; DECKHUT, Charlotte Pooley; EDWARDS, James P.; GHOSH, Brahmananda; KREUTTER, Kevin; LI, Gang; TICHENOR, Mark S.; VENABLE, Jennifer D.; WEI, Jianmei; WIENER, John J. M.; WU, Yao; XIAO, Kun; ZHANG, Feihuang; ZHU, Yaoping; (528 pag.)WO2017/100662; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

191348-14-8, name is 2-Iodo-4-methoxyaniline, 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. Recommanded Product: 191348-14-8

General procedure: Step B: Pyridine (1.5 mmol) was added to the o-iodo derivative as prepared above (1 mmol) in DCM (5 mL) at 0 C under nitrogen atmosphere. To this was added methane/p-toluene sulfonyl chloride (1.2 mmol) slowly at 0 C. Then, the reaction mixture was stirred at room temperature for 5-6 h. After completion of the reaction (monitored by TLC), the reaction mixture was diluted with ethyl acetate (30 mL), washed with 2N HCl solution (10 mL) followed by brine solution (20 mL), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography using ethyl acetate-hexane to give the desired product 2.

The synthetic route of 191348-14-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Rambabu; Raja, Guttikonda; Yogi Sreenivas; Seerapu; Lalith Kumar; Deora, Girdhar Singh; Haldar, Devyani; Rao, M.V.Basaveswara; Pal, Manojit; Bioorganic and Medicinal Chemistry Letters; vol. 23; 5; (2013); p. 1351 – 1357;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, molecular formula is C6H3ClFI, 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. Computed Properties of C6H3ClFI

To a solution of 2-chloro-4-fluoro-l-iodo-benzene (3.6 g, 14.3 mmol) and 3-trifluoromethyl-lH-pyrazole (1.9 g, 14.4 mmol) in N,N-dimethylformamide (40 mL) was added potassium carbonate (2.4 g, 17.2 mmol), and the resulting mixture was heated at 135 C for 12 h. The reaction mixture was cooled to room temperature, poured in cold water (80 mL) and extracted with dichloromethane (2 x 40 mL). The combined organic extracts were dried (Na2S04) and concentrated under reduced pressure. The residue was purified by flash column chromatography on silica gel eluted with 10% ethyl acetate in hexanes to afford the title compound (4.2 g) as a white solid. lH NMR delta 10.4 (s, 1H), 7.88 (m, 2H), 7.80 (d, 1H), 7.27 (m, 1H), 6.68 (d, 1H). MS (AP+) 373 amu.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 101335-11-9, its application will become more common.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; BEREZNAK, James, Francis; GUTTERIDGE, Steven; TAGGI, Andrew, Edmund; REDDY, Ravisekhara, P.; CAMPBELL, Matthew, James; KAR, Moumita; DESAEGER, Johan, A., J.; WO2014/4064; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com