Category: 401-81-0

Adding a certain compound to certain chemical reactions, such as: 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, 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 401-81-0, Safety of 1-Iodo-3-(trifluoromethyl)benzene

Dioxane (100 mL) was purged with nitrogen gas for 10 min. Phenanthrolene ( 1.0 g) and copper (I) iodide (1.0 g) were added to the dioxane, the suspension was allowed to stir under a nitrogen atmosphere for 5 min, and then cesium carbonate ( 18.72 g, 57.45 mmol), dimethyl malonate (5.46 g, 50.6 mmol), and l-iodo-3-(trifluoromethyl)benzene (12.5 g, 46.0 mmol) were added. The reaction mixture was heated to reflux for 18 h and then cooled to room temperature. Aqueous 1 N HC1 was added to the reaction mixture, the layers were separated, and the aqueous layer was extracted with ethyl acetate (3 x 100 mL). The combined organic layers were dried over magnesium sulfate and filtered. Celite diatomaceous filter aid (5 g) was added to the filtrate, and the resulting suspension was concentrated under reduced pressure at 50 C to yield a solid consisting of the crude product adsorbed onto Celite. This solid was purified by silica gel chromatography eluting with a gradient of 100% hexanes to 25% ethyl acetate in hexanes to yield 7.36 g (58.0%) of the title product. NMR (CDC13) delta 7.59-7.65 (m, 3H), 7.49 (t, 1H), 4.70 (s, 1H), 3.76 (s, 6H).

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-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; ZHANG, Wenming; ANNIS, Gary David; WO2013/90547; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 401-81-0, A common heterocyclic compound, 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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.

Step C: Preparation of 1 ,3-dimethyl 2-[3-(trifluoromethyl)phenyl]propanedioateDioxane (100 mL) was purged with nitrogen gas for 10 minutes. Phenanthrolene (1.0 g) and copper (I) iodide (1.0 g) were added to the dioxane, the suspension was allowed to stir under a nitrogen atmosphere for 5 minutes, and then cesium carbonate (18.72 g, 57.45 mmol), dimethyl malonate (5.46 g, 50.6 mmol), and l-iodo-3-(trifluoromethyl)benzene (12.5 g, 46.0 mmol) were added. The reaction mixture was heated to reflux for 18 hours and then cooled to room temperature. Aqueous 1 N HC1 was added to the reaction mixture, the layers were separated, and the aqueous layer was extracted with ethyl acetate (3 x 100 mL). The combined organic layers were dried over magnesium sulfate and filtered. Celite diatomaceous filter aid (5 g) was added to the filtrate, and the resulting suspension was concentrated under reduced pressure at 50 C to yield a solid consisting of the crude product adsorbed onto Celite. This solid was purified by silica gel chromatography eluting with a gradient of 100% hexanes to 25% ethyl acetate in hexanes to yield 7.36 g (58.0%) of the title product. .H NMR (CDC13) delta 7.59-7.65 (m, 3H), 7.49 (t, 1H), 4.70 (s, 1H), 3.76 (s, 6H).

The synthetic route of 401-81-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; PAHUTSKI, Thomas, Francis., Jr.; WO2012/92115; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 401-81-0, A common heterocyclic compound, 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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: 4-Iodoanisole (0.813 mmol, 200 mg), bis(pinacolato)diboron (1.219 mmol, 309 mg) were dissolved in 3 mL of dmf followed by copper ferrite nanoparticles (5mol% with respect to 4-iodoanisole) and potassiumtert-butoxide (1.219 mmol, 137 mg) were added to a 10 mLcapped vial and stirred at RT for time indicated. After stirring, the mixture was diluted with diethyl ether and filtered through celite bed. The filtrate was extracted with water (3 times) and the organic phase was dried over anhydrous MgSO4. The crude product was subjected to analyze by GC-MS. The conversion yield is accurately measured based on the consumption of 4-iodoanisole and the side product formed due to protodeiodination.

The synthetic route of 401-81-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Mohan, Balaji; Kang, Hyuntae; Park, Kang Hyun; Catalysis Communications; vol. 85; (2016); p. 61 – 65;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 401-81-0, 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.

General procedure: A Schlenk tube was charged with MCM-41-2N-CuI (66 mg,0.03 mmol), MeCSNH2(75 mg, 1.0 mmol), Cs2CO3(978 mg,3.0 mmol), and aryl halide (2.5 mmol). The tube was evacuated andbackfilled with argon. Then, DMSO-H2O (1 ml/0.5 ml) was addedunder argon. The tube was sealed, and the reaction mixture wasstirred at 120C for 24-48 h. The reaction mixture was cooled toroom temperature, diluted with ethyl acetate (10 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 thenext run. The filtrate was concentrated under reduced pressureand the residue was purified by flash column chromatography onsilica gel (petroleum/ethyl acetate = 50:1 to 7:1) to provide thedesired product.

The chemical industry reduces the impact on the environment during synthesis 1-Iodo-3-(trifluoromethyl)benzene. I believe this compound will play a more active role in future production and life.

Reference:
Article; Cai, Mingzhong; Yao, Ruiya; Chen, Lin; Zhao, Hong; Journal of Molecular Catalysis A: Chemical; vol. 395; (2014); p. 349 – 354;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, 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. category: iodides-buliding-blocks

Add triethylamine (6. 2 mL, 44 mmol), copper (I) iodide (120. 3 mg, 1. 10 mmol) and bis (triphenylphosphine) palladium (II) dichloride (386 mg, 0. 55 mmol) to a solution of 3-bromo-5-ethynylpyridine, (prepared essentially as described in PREPARATION 23), (2. 0 g, 11 mmol) and 1-iodo-3-trifluoromethylbenzene (1. 53 mL, 11 mmol) in ethyl acetate (12 mL). Stir at room temperature for 18 h. Concentrate and purify the residue by silica gel chromatography, eluting with 100 : 0 to 100 : 50 hexanes : ethyl acetate to give the title compound (2. 1 g, 61%). 1H NMR (300 MHz, CDCl3) 6 7. 52 (t, J = 8. 0 Hz, 1H), 7. 64 (d, J = 8. 0 Hz, 1H), 7. 71 (d, J = 8. 0 Hz, 1H), 7. 80 (br s, 1H), 7. 98 (t, J = 2. 2 Hz, 1H), 8. 64 (d, J = 2. 2 Hz, 1H), 8. 68 (d, J = 2. 2 Hz, 1H) ; MS (ES) : m/z = 326 [M+H] +.

The synthetic route of 1-Iodo-3-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/94822; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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. Safety of 1-Iodo-3-(trifluoromethyl)benzene

The mixture of Intermediate-51a (150mg, 0.45mmol), l-iodo-3(trifluoromethyl)benzene (0.18g,0.68 mmol) and CS2CO3 (0.22 g, 0.68 mmol) in toluene (7mL) was degassed for 15 min by purging nitrogen followed by addition of bis (tri-tert-butylphosphine palladium(O) (11.53mg, 0.023 mmol) and tris dibenzylidene acetone dipalladium (0)(20.66mg,0.023 mmol). The reaction mixture was heated to 110C and further maintained for 20 hr at the same temperature. The reaction mixture was cooled to room temperature and progress of reaction monitored by TLC. The mixture was diluted with ethyl acetate, filtered through celite and concentrated under vacuum to give crude compound. This crude compound was further purified by flash chromatography using a mixture of 20% ethylacetate in hexane (0.17g, 79%).Ethereal HCl (2 mL) was added and stirred for 10 min. The solvent was evaporated and solid washed by diethyl ether (2 mL) followed by «-pentane (2 ml), dried to get HCl salt of title compound.m/z 477.2; *H NMR (400 MHz, DMSO-d6): delta 9.64 (bs, IH), 9.10 (bs, IH), 8.24 (d, 7=8.4 Hz, IH), 8.03 (t, 7=8.8 Hz, 2H), 7.89 (d, 7=7.2 Hz, IH), 7.63-7.48 (m, 6H), 7.37(d, 7=7.6 Hz, IH), 6.93 (d, 7=7.2 Hz, IH), 6.80-6.77 (m, 3H), 5.34 (m, lH), 4.28 (m, 1H),3.85 (m, lH), 3.47-3.10 (m, 3H), 2.03 (m, 2H), 1.67 (d, 7=6.8 Hz, 3H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 401-81-0, its application will become more common.

Reference:
Patent; LUPIN LIMITED; SHUKLA, Manojkumar, Ramprasad; ANKUSH, Sarde, Gangaram; VIPUL, Pachpute, Dilip; KULKARNI, Sanjeev, Anant; PALLE, Venkata, P.; KAMBOJ, Rajender, Kumar; WO2012/127385; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 401-81-0, A common heterocyclic compound, 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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: To a solution of aryl iodide (10 mmol, 1.0 equiv.) in THF (10 mL, 1.0 M) was added 2-propyn-1-ol (1.24 mL, 1.2 equiv.), diisopropylamine (1.68 mL, 1.2 equiv.), PdCl2(PPh3)2 (0.3 mmol, 3 mol%) andCuI (0.5 mmol, 5 mol%). The resulting solution changed colour from yellow to orange and finallybrown in two minutes. The reaction mixture was heated at 50 C and stirred until completeconsumption of the aryl iodide was observed (tlc, 2 h). After filtering the crude material over a padof silica (5 g) and evaporation of the solvent the crude material (1H-NMR) was purified by silica column chromatography (eluent 10% EtOAc in pentanes, Rf = 0.41). After removal of the volatiles,the desired hydroxyl product was typically isolated as yellow oil with a purity > 98% (by 1H-NMR)and was used directly in the next step. Copies of NMR spectra are provided in the electronicsupplementary information.

The synthetic route of 401-81-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Donnelly, Kian; Zhang, Huan; Baumann, Marcus; Molecules; vol. 24; 20; (2019);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, 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 401-81-0, Formula: C7H4F3I

General procedure: The N-nucleophile (1.47 mmol), CuI (Sigma-Aldrich, 99.999% purity, 0.147 mmol), MnF2 (Sigma-Aldrich, 98% purity, 0.441 mmol), KOH (2.94 mmol), the aryl halide (2.21 mmol), trans-1,2-diaminocyclohexane (0.294 mmol) and water (0.75 mL) were added to a reaction vial and a screw cap was fitted to it. The reaction mixture was stirred under air in a closed system at 60C for 24 h. After cooling to room temperature, the mixture was diluted with dichloromethane and filtered through a pad of Celite. The combined organic extracts were dried with anhydrous Na2SO4 and the solvent was removed under reduced pressure. The crude product was purified by silica-gel column chromatography to afford the N-arylated product. The identity and purity of known products was confirmed by 1H and 13C NMR spectroscopic analysis.

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; Teo, Yong-Chua; Yong, Fui-Fong; Lim, Gina Shiyun; Tetrahedron Letters; vol. 52; 52; (2011); p. 7171 – 7174;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene, molecular formula is C7H4F3I, 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. Safety of 1-Iodo-3-(trifluoromethyl)benzene

General procedure: A mixture of thiol (0.5 mmol), aryl halide (0.6mmol), CuI (5 mol%, 4 mg), DABCO (10 mol%, 5.6 mg) K2CO3(2 equiv, 138 mg) and DME (3 ml) were added to an oven-dried sealed tube equipped with a stirring bar under nitrogen. The sealed tube was stirred in a preheated oil bath at 120 oC for 12 h. After being cooled to room temperature, the mixture was diluted with ethyl acetate(30 ml) and washed with saturated aqueous NaCl solution (3 x 15 ml).The organic phase was dried with anhydrous Na2SO4,filtered, and the solvent was removed under vacuum. The crude residue was purified by column chromatography on silica gel using ethyl acetate/hexanes as the eluent to give the desired sulphides.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 401-81-0, its application will become more common.

Reference:
Article; Thomas, Anns Maria; Asha, Sujatha; Sindhu; Anilkumar, Gopinathan; Tetrahedron Letters; vol. 56; 47; (2015); p. 6560 – 6564;,
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. 401-81-0, name is 1-Iodo-3-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: iodides-buliding-blocks

General procedure: Catalyst 1 (prepared according Ref.15a, 7.1 mg,0.05 mequiv of Pd) was added to a solution of aryl iodide (4 mmol,1.0 equiv), methyl acrylate (0.72 mL, 8 mmol, 2.0 equiv), Et3N (0.67 mL,4.8 mmol, 1.2 equiv) in a mixture of toluene (6.7 mL), DMF (3.3 mL) and H2O(0.1 mL). The reaction mixture was heated at 100 C for 20 h. After coolingto rt, 1 was filtered off under vacuum. The mixture of solvents wasconcentrated under vacuum and the residue was purified by flashchromatographyon silica gel to afford pure alkenes after drying under,vacuum (0.1 mbar).

The synthetic route of 401-81-0 has been constantly updated, and we look forward to future research findings.