Author: Jessica.F

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. 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C7H4F3I

General procedure: To a resealable Schlenk tube were added indole (1.0 mmol), K3PO4 (0.424 g, 2.0 mmol), and MCM-41-2N-CuI (88 mg, 0.04 mmol), and the reaction vessel was fitted with a rubber septum. The vessel was evacuated and back-filled with argon and this evacuation/back-fill procedure was repeated one additional time. The aryl halide (1.2 mmol) and toluene (2 mL) were then added under a stream of argon. The reaction tube was quickly sealed and the contents were stirred while heating in an oil bath at 110 C for 24-48 h. After completion of the reaction, the reaction mixture was cooled to room temperature, diluted with ethyl acetate (5 mL), and filtered. The MCM-41-2N-CuI complex was washed with distilled water (2×5 mL), ethanol (2×5 mL), and Et2O (2×5 mL) and reused in the next run. The filtrate was concentrated under reduced pressure and the residue was purified by flash column chromatography on silica gel (petroleum/ethyl acetate=50:1 to 4:1) to provide the desired product.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 401-81-0.

Reference:
Article; Xiao, Ruian; Zhao, Hong; Cai, Mingzhong; Tetrahedron; vol. 69; 26; (2013); p. 5444 – 5450;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

39998-81-7, name is 2-Fluoro-4-iodo-1-methylbenzene, 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. SDS of cas: 39998-81-7

Methyl-2-fluoro-4-iodo benzoate (Reagent G) A solution of 2-fluoro-4-iodo toluene (5 g, 26.6 mmol) in pyridine (2 mL) and water (20 mL) was treated with potassium permanganate (16.6 g, 105 mmol) and heated at 150 C. overnight. The reaction mixture was then cooled to room temperature and filtered and the filtrate was extracted with hexane. The aqueous phase was acidified with 10% hydrochloric acid and extracted with ethyl acetate. The organic phase was dried over anhydrous sodium sulfate, filtered and evaporated in vacuo. The residue was dissolved in 20 mL of methanol, treated with concentrated sulfuric acid (1 mL) and refluxed overnight. The volatiles were distilled off in vacuo and the residue was dissolved in diethyl ether, washed with brine, dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to an oil. Flash column chromatography over silica gel (230-400 mesh) using 10% ethyl acetate in hexane as the eluent afforded the title compound as an oil (0.26 g, 5%). 1H NMR (300 MHz, CDCl3):delta 7.60 (m, 4H), 3.93 (s, 3H).

The synthetic route of 39998-81-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Allergan Sales, Inc.; US6252090; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 25252-00-0, 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 25252-00-0 as follows.

Part C. 3′-(1-benzyl-6-cyano-1H-indol-3-ylmethyl)-4-carbamoyl-biphenyl-2-carboxylic acid benzyl ester:; 2-Bromo-5-iodobenzoic acid (6.54 g, 20.0 mmol) was dissolved in DMF (70 mL). Potassium bicarbonate (2.2 g, 22.0 mmol) was added, followed by benzyl bromide (2.8 mL, 22.0 mmol). The mixture was stirred at rt under N2 for 12 h. The reaction mixture was poured into water and extracted with EtOAc. The combined organic solution was washed with brine, dried over MgSO4, and concentrated and dried to give 9.05 g of the benzyl ester. The ester (2.3 g, 7.69 mmol), Zn(CN)2 (1.3 g, 11.5 mmol), and Pd[PPh3]4 were dissolved together in 25 mL of DMF. The mixture was de-gassed and heated at 90 C. for 4 h. Reaction mixture was concentrated and purified by chromatography (silica gel, 5% EtOAc in hexane) to give 1.8 g of the benzonitrile. MS: 316.0, 317.9 (M+1)+. The benzonitrile (1.4 g, 4.4 mmol) was dissolved in 15 mL of DMF. The reaction mixture was cooled at 0 C. Potassium carbonate (0.20 g, 1.45 mmol) was added, followed by dropwise addition of 30% hydrogen peroxide solution (1.2 mL). The cooling bath was removed and the mixture was stirred at rt for 12 h. The reaction was quenched with aqueous NaHSO3 and water. The formed precipitate was filtered and dried to give 1.1 g of the desired amide. MS: 334.2, 336.3 (M+1)+. A mixture of the resulting amide (0.2 g, 0.6 mmole), bis(pinacolato)diboron (0.228 g, 0.9 mmol) and anhydrous KOAc (0.18 g, 1.8 mmol) in 2 mL of 1,4-dioxane was purged with argon, then (1,1′)-bis(diphenylphosphino)ferrocene)palladium(II) chloride (20 mg, 0.024 mmol) was added. The resulting mixture was heated in a sealed tube in a microwave reactor at 100 C. for 2 h then left standing overnight at rt. The reaction was diluted with water and extracted 3× with EtOAc. The combined extracts were washed with brine, dried over Na2SO4, filtered and evaporated in vacuo. Chromatography on silica gel (hexane/ethyl acetate 1:1) provided the boronate (0.13 g, 57%). A mixture of this compound, the compound of Part B (0.1 g, 0.25 mmol), and K3PO4 (0.11 g, 0.5 mmol) in 5 mL dioxane was degassed and then treated with tetrakis(triphenylphosphine)palladium(20 mg, 0.017 mmol). The resulting mixture was heated in a 95-100 C. oil bath under N2 for 2 h, then stirred at rt overnight. The reaction mixture was diluted with brine and extracted 3× with EtOAc. The combined extracts were washed with brine then dried over anhydrous Na2CO3, filtered and evaporated. Chromatography on silica gel (hexane/ethyl acetate 1:1) provided the product (0.12 g, 83%) as a light yellow foam. 1H NMR (400 MHz, CDCl3) delta ppm 4.07 (s, 2H) 4.90 (s, 2H) 5.23 (s, 2H) 6.91 (d, J=6.15 Hz, 2H) 7.05 (m, 3H) 7.20 (m, 6H) 7.29 (m, 5H) 7.42 (d, J=7.91 Hz, 1H) 7.51 (d, J=10.99 Hz, 2H) 7.98 (dd, J=8.13, 1.98 Hz, 1H) 8.19 (d, J=2.20 Hz, 1H). LC/MS m/z 576.16 (M+H)+.

According to the analysis of related databases, 25252-00-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Smallheer, Joanne M.; Corte, James R.; US2005/228000; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 328-73-4, 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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: In an open round-bottomed flask containing deionised water (20?25 mL), azido-alkyne (1, 1.0 equiv), aryl iodide (2, 2.0 equiv), cuprous oxide nanomaterials (15 mol percent), and Cs2CO3 (2.0 equiv) were added and stirred vigorously under sonication for 1?1.5 h at 80 °C, making sure that no halides escaped during the reaction. After that ethyl acetate was added in it and the mixture was centrifuged to separate the nanocatalyst. Aqueous phase was then again extracted with ethyl acetate repeatedly. Column chromatography afforded pure product (3a?k). The nanoparticles were washed with ethanol water(3) and dried under vacuum before reuse.

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, 1-Iodo-3,5-bis(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Chatterjee, Nivedita; Pal, Rammyani; Sarkar, Swarbhanu; Sen, Asish Kumar; Tetrahedron Letters; vol. 56; 25; (2015); p. 3886 – 3889;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 450412-28-9,Some common heterocyclic compound, 450412-28-9, name is 1-Bromo-3-chloro-2-iodobenzene, molecular formula is C6H3BrClI, 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.

A round bottom flask was charged with 13.45 g of phenylboronic acid, 110.29 mmol) was added dropwise a solution of 1-bromo-3-chloro-2-iodobenzene (35 g, 110.29 mmol), Pd (PPh3) 4 (1.27 g, 1.10 mmol), NaOH (4.41 g, 110.29 mmol), THF (485 mL) and water (243 mL). Then, the mixture is heated under reflux at 80 C . When the reaction is complete, dilute with distilled water at room temperature and extract with methylene chloride and water. The organic layer was dried over MgSO4 and concentrated. The resulting compound was purified by silicagel column and recrystallized to obtain 18.59 g of the product. (Yield: 63%)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-3-chloro-2-iodobenzene, its application will become more common.

Reference:
Patent; DUK SAN NEOLUX CO., LTD.; KIM, Hyo Jin; PARK, Nam Jin; KIM, Seul Gi; HWANG, Sun Pil; (46 pag.)KR2017/95602; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. Computed Properties of C4H8I2

General procedure: Under N2 atmosphere, LHMDS (1 M in THF, 3.0 equiv) was added to a cooled solution (0 C) of tricyclic lactam (1.0 equiv) dissolved in THF (6 mL). After stirring for 1 h at 0 C, an excess of alkyl halide (3.0 equiv for methyl iodide and 5.0 equiv for ethyl iodide) was added. For the introduction of five and six membered spirocyclic rings 1,4-diiodobutane or 1,5-diiodopentane (1.0 equiv) was added at 0 C. The solution was stirred for a further 3 h at 0 C. Completion of the conversion was confirmed by TLC. Saturated NaCl solution (10 mL) was then added and the mixture was extracted with EtOAc (3 × 10 mL). The organic layer was washed with NaCl solution (10 mL) and water (10 mL) and the aqueous layer was reextracted with EtOAc (2 × 10 mL). The combined organic layers were dried (Na2SO4), filtered, and the solvent was evaporated in vacuo and the residue was purified by FC.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 628-21-7, its application will become more common.

Reference:
Article; Sarkar, Soumya; Schepmann, Dirk; Wuensch, Bernhard; Tetrahedron Asymmetry; vol. 22; 13; (2011); p. 1411 – 1422;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 116632-39-4, These common heterocyclic compound, 116632-39-4, name is 5-Bromo-2-iodotoluene, 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.

(1) 4-Bromo-4′-fluoro-2-methylbiphenyl 4-Bromo-1-iodo-2-methylbenzene (10.5 g, 35.4 mmol) was dissolved in 1,2-dimethoxyethane (100 mL), and (4-fluorophenyl)boronic acid (7.4 g, 52.9 mmol), [1,1′-bis(diphenylphosphino)ferrocene]palladium dichloride-dichloromethane adduct (1.5 g, 1.84 mmol) and potassium phosphate hydrate (18.8 g, 88.6 mmol) were added, followed by stirring at room temperature for 16 hours under a nitrogen atmosphere. After the insoluble materials in the reaction solution were filtered off, the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (Moritex Corporation, elution solvent:hexane), and a fraction corresponding to the Rf value=0.60 (hexane) by thin layer chromatography was concentrated under reduced pressure to afford the title compound (5.1 g, 19.2 mmol) as a colorless oil (yield 54%). 1H-NMR (500 MHz, CDCl3) delta: 7.42 (1H, s), 7.36 (1H, d, J=8 Hz), 7.27-7.21 (2H, m), 7.13-7.04 (3H, m), 2.22 (3H, s).

The synthetic route of 116632-39-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DAIICHI SANKYO COMPANY, LIMITED; US2011/112103; (2011); 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. 1643-29-4, name is 3-(4-Iodophenyl)propanoic acid, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H9IO2

General procedure: HOBT (1.2 equiv.) was added to an ice-cooled solution of EDCI (1.2 equiv.) in anhydrous DMF (10 mL) under N2. The resulting solution was allowed to stir for 10 min. at 0 C, followed by the addition of the appropriate acid 7a-7l (1.2 equiv.) and DIPEA (2.5 equiv.). The resulting solution was stirred for another 15 min at 0 C, after which a solution of amine 6 (1.0 equiv.) in anhydrous DMF (5 mL) was added. The resulting reaction mixture was allowed to stir first at 0 C for 30 mins, then at rt for 5 h. The reaction mixture was then evaporated to dryness under vacuum. Saturated NaHCO3 solution (10 mL) was then added to the resulting crude followed by extraction of the aqueous layer using dichloromethane (3 x 15 mL). The combined organic layer was dried over Na2SO4 and evaporated to dryness under vacuum to afford the corresponding amides which were purified using flash column chromatography (30 – 50 % ethyl acetate -petroleum ether).

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; Kapadia, Nirav; Ahmed, Shahrear; Harding, Wayne W.; Bioorganic and Medicinal Chemistry Letters; vol. 26; 14; (2016); p. 3216 – 3219;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 628-77-3, These common heterocyclic compound, 628-77-3, name is 1,5-Diiodopentane, 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.

A solution of oxindole (25 g, 0.19 mol) in anhydrous tetrahydrofuran (800 cm3) was cooled to -20 C. then n-butyllithium (2.5M in hexanes, 152 cm3, 0.38 mol) was added slowly followed by N,N,N’,N’-tetramethylethylenediamine (51 cm3, 0.38 mol,).. After 15 min. 1,5-dilodopentane (174 g, 0.54 mol) was added slowly and the mixture was allowed to warm to room temperature.. After stirring for 16 h. saturated aqueous ammonium chloride solution (1L) and EtOAc (1L) were added.. After 15 min., the layers were separated and the aqueous phase was extracted with EtOAc (*2).. The combined organic layers were extracted with hydrochloric acid (1N), then washed with brine (500 cm3), dried (MgSO4), and concentrated to obtain an oil.. The oil was triturated with hexane (200 cm3) and benzene (20 cm3).. The precipitate was collected and dried in vacuo to obtain the subtitled compound (26.3 g, 69.6%) as colorless crystals: mp 110-114 C.; 1H NMR (DMSO-d6) delta 1.67 (m, 10H), 6.84 (d, 1H, J=8 Hz) 6.94 (t, 1H, J=8 Hz), 7.17 (t, 1H, J=8 Hz), 7.44 (d, 1H, J=8 Hz), 10.3 (S, 1H).

Statistics shows that 1,5-Diiodopentane is playing an increasingly important role. we look forward to future research findings about 628-77-3.

Reference:
Patent; American Home Products Corporation; Ligand Pharmaceuticals, Inc.; US6355648; (2002); B1;,
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. 55406-53-6, name is 3-Iodoprop-2-yn-1-yl butylcarbamate, A new synthetic method of this compound is introduced below., Computed Properties of C8H12INO2

EXAMPLESA solution is prepared in Dowanol TPM (tripropylene glycol methyl ether), containing 10% by weight of iodopropargyl butylcarbamate, 5% by weight of Octasoligen-Cobalt 8 (Borchers, Langenfeld, Germany) and 5% by weight of the stabilizer specified in Table 1. The compositions are stored at 40 C. The amount of IPBC was determined by means of HPLC at the beginning and after two weeks.

The synthetic route of 55406-53-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Uhr, Hermann; US2009/36555; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com