Category: 4028-63-1

Application of 4028-63-1, The chemical industry reduces the impact on the environment during synthesis 4028-63-1, name is 2,4,6-Trimethyliodobenzene, I believe this compound will play a more active role in future production and life.

General procedure: Aryl iodide (1 mmol), nucleophile (0.8-1.2 mmol), tris-(2-furyl)-phosphine (TFP) (10 mol percent), tris-dibenzylideneacetonedipalladium (0) (Pd2dba3) (2.5 mol percent), base (2 mmol) and MeCN (20 mL) were combined in a Schlenk tube. After two freeze-pump-thaw cycles, allene gas (0.5 atm) was charged into the Schlenk tube, the mixture thawed and then heated for 16-24 h at 70-80°C with magnetic stirring. After cooling to room temperature and venting excess allene, DCM (10 mL) was added, the mixture filtered, and the filtrate evaporated in vacuo. Column chromatography of the residue afforded the product.

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, 2,4,6-Trimethyliodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Dondas, H. Ali; Hempshall, Aiden; Narramore, Sarah; Kilner, Colin; Fishwick, Colin W.G.; Grigg, Ronald; Tetrahedron; vol. 72; 10; (2016); p. 1316 – 1329;,
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. 4028-63-1, name is 2,4,6-Trimethyliodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 4028-63-1

General procedure: To a stirred solution of aryl halide (1.2mmol) and [Pd(pp3S4)(dba)] (1mol percent) in isopropanol (2.5ml) was added nitrogen/oxygen nucleophile (1mmol) followed by Cs2CO3 (2mol percent) in the atmosphere of air. The mixture was heated to 80°C and the progress of the reaction was monitored by TLC. After completion, the solvent was evaporated through rotavapour and the crude mixture was washed with dichloromethane-H2O and the organic phase was separated and dried over Na2SO4. The dichloromethane was evaporated followed by flash column purification on silica gel of the crude to obtain the pure products. The products were characterized using 1H, 13C NMR spectroscopy and GC?MS spectroscopy. The characterization data were in good agreement with those described in the literature.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Majumder, Arpi; Gupta, Ragini; Mandal, Mrinmay; Babu, Madhu; Chakraborty, Debashis; Journal of Organometallic Chemistry; vol. 781; (2015); p. 23 – 34;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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.

tert-Butyllithium (9.0 mL of a 1.7 mol/l solution in n-pentane, 15.3 mmol)was added to iodomesitylene (10) (1.51 g, 6.14 mmol) in Et2O (20 mL) at ?78 °C under inertatmosphere. After 30 min, CuCN (273 mg, 3.07 mmol) was added and the suspension stirred at?60 °C for 2 h. The reaction mixture was then treated with nitrobenzene (0.94 mL, 9.12 mmol)and allowed to warm up to room temperature overnight. An aqueous solution of NH3 (12.5percentw/w, 80 mL) was slowly added and the resulting residue was extracted with MTBE (3 x 50 mL).The combined organic layers were washed with water (50 mL) and brine (50 mL), dried overMgSO4, filtered, and the solvent was removed in vacuum. The product 11 could be obtained aftercolumn chromatography (SiO2, n-hexane, Rf 0.43) as a colorless solid (542 mg, 2.27 mmol,74percent), mp 98 °C (ref.27 99?100 °C). 1H NMR (300 MHz, CDCl3): delta 6.94 (s, 4 H), 2.34 (s, 6 H),1.87 (s, 12 H) ppm. 13C{1H} NMR (75 MHz, CDCl3): delta 137.0 (2 C), 136.0 (2 C), 135.5 (4 C),128.2 (4 CH), 21.1 (2 CH3), 19.8 (4 CH3) ppm. IR (ATR): 2997 (w), 2938 (m), 2916 (m), 1470(m), 1436 (m), 1375 (m), 1004 (m), 852 (s), 595 (m) cm?1. MS (EI, 70 eV), m/z (percent): 238 (99)[M+], 223 (100), 208 (33), 193 (25). Anal. calcd. for C18H22 (238.37): C 90.70, H 9.30; found C90.73, H 9.34.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Behler, Florian; Wickleder, Mathias S.; Christoffers, Jens; ARKIVOC; vol. 2015; 2; (2014); p. 64 – 75;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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: A 10 mL flask equipped with a Teflon valve was charged with a magnetic stir bar, CuI (2 mg, 1molpercent), Heteroarylamine (1.5 mmol), KOtBu (224 mg, 2.0 mmol), solid aryl halides (1.0 mmol). The tube was evacuated and backfilled with argon. Under a counter flow of argon, dioxane (1.5mL), aryl halides (1.0 mmol, if liquid) were added by syringe. The tube was sealed. The reaction mixture was allowed to stir at 110 °C (X=I) or 130 °C (X= Br) for 24 h. Then the mixture was cooled to room temperature and added 5.0 mL brine. Subsequently, the mixture was extracted with ethyl acetate. The organic layers were collected, dried over Na2SO4, filtered and the solvent was removed under vacuum. The residue was purified by column chromatography on silica gel.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Deping; Kuang, Daizhi; Zhang, Fuxing; Liu, Yang; Ning, Shunhua; Tetrahedron Letters; vol. 55; 51; (2014); p. 7121 – 7123;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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.

2,4,6-trimethyliodobenzene (12 mmol, 3 equiv), elemental selenium (12 mmol, 3 equiv), 5-methylbenzoxazole (4 mmol, 1 equiv), Cu(OAc) 2 (at room temperature) 0.4 mmol), ammonium hydrogencarbonate (12 mmol, 3 equiv) was added to the reaction tube, then filled with nitrogen, and replaced three times. Under a nitrogen reaction environment, 20 mL of DMF reaction solvent was then added, and the mixture was stirred at a reaction temperature of 140 ° C for 24 hours. After monitoring the reaction by thin layer chromatography, the reaction mixture was cooled, then diluted with ethyl acetate, and the diluted solution was transferred to a separating funnel, and extracted with saturated brine to separate the aqueous and organic phases, and then acetic acid. The aqueous phase was extracted three times with ethyl acetate. The organic phase was combined, 25 g of anhydrous sodium sulfate was added, and the mixture was allowed to stand for 30 min, and the filter cake was washed three times with 50 mL of ethyl acetate each time, then the solvent was spun off, and the product was separated by column chromatography. Deprotection: petroleum ether: diethyl ether = 98:2), yield 90percent, product weight 1.191 g.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wenzhou Medical University; Wu Ge; (9 pag.)CN108484518; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 4028-63-1,Some common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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 room temperature,A mixture of 2,4,6-trimethyliodobenzene (1.2 mmol, 3 equiv)Elemental selenium (1.2 mmol, 3 equiv),5-phenyl-1,3,4-oxadiazole (0.4 mmol, 1 equiv),Cu (OAc) 2 (0.04 mmol),Potassium carbonate (1.2 mmol, 3 equiv) was added to the reaction tube,Then filled with nitrogen, and replaced three times, in the nitrogen reaction environment,Then, 2 mL of DMF was added to the reaction solvent and stirred at 140 ° C for 24 h.After the reaction was monitored by thin layer chromatography, the reaction mixture was cooled,Then diluted with ethyl acetate, and the diluted solution was transferred to a separatory funnel,Extracted with saturated brine, separated from the aqueous phase and organic phase, and then extracted with ethyl acetate 3 times,The organic phases were combined, 5 g of anhydrous sodium sulfate was added,Wash the filter cake with 5 mL of ethyl acetate each time 3 times, then spin off the solvent,The product was isolated by column chromatography (eluent: petroleum ether: ether = 98: 2)The product was a yellow solid, yield 90percent, product weight 123 mg.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wenzhou Medical University; Wu Ge; (23 pag.)CN107056727; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 4028-63-1, These common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, 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 reaction was generally performed with 2.0 equivalents of TfOH. m-CPBA (65%active oxidant, 2.6 mmol) and aryl iodide (2.3 mmol) were dissolved in DCM (20 mL)in a sealed tube. The arene (2.6 mmol) was added and the solution was cooled to 0 oC,followed by dropwise addition of TfOH (4.6 mmol), and resulted in a colouredsolution. The reaction mixture was stirred for about 2 h, subsequently concentratedunder vacuum. Et2O was added and the mixture was stirred at room temperature for30 mins to precipitate out an off-white solid.

Statistics shows that 2,4,6-Trimethyliodobenzene is playing an increasingly important role. we look forward to future research findings about 4028-63-1.

Reference:
Article; Liu, Qi-Sheng; Wang, De-Yin; Yang, Jin-Fei; Ma, Zhong-Yi; Ye, Mengchun; Tetrahedron; vol. 73; 26; (2017); p. 3591 – 3595;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, 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. Computed Properties of C9H11I

1.0 mmol of 2,4,6-trimethyliodobenzene,1.2 mmol sodium azide,0.15 mmol DBUAnd 0.1mmol of copper acetate were sequentially added to a reaction flask equipped with 3mL of dimethyl sulfoxide,The reaction mixture was stirred at 95 ¡ã C for 2h,TLC was followed until the reaction was complete,A few drops of aqueous ammonia were added to the reaction mixture,Then extracted with ethyl acetate (10 mL ¡Á 3),Then washed once with saturated saline,dry,Suction filtration,Remove the solvent,Purification by column chromatography gave the desired product,Yield 78percent.

The synthetic route of 2,4,6-Trimethyliodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Henan Normal University; Jiang Yuqin; Zhao Yaru; Ma Suhao; Li Xingfeng; Dong Wenpei; Xu Guiqing; (10 pag.)CN106588693; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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: A 10 mL flask equipped with a Teflon valve was charged with a magnetic stir bar, CuI (2 mg, 1molpercent), Heteroarylamine (1.5 mmol), KOtBu (224 mg, 2.0 mmol), solid aryl halides (1.0 mmol). The tube was evacuated and backfilled with argon. Under a counter flow of argon, dioxane (1.5mL), aryl halides (1.0 mmol, if liquid) were added by syringe. The tube was sealed. The reaction mixture was allowed to stir at 110 ¡ãC (X=I) or 130 ¡ãC (X= Br) for 24 h. Then the mixture was cooled to room temperature and added 5.0 mL brine. Subsequently, the mixture was extracted with ethyl acetate. The organic layers were collected, dried over Na2SO4, filtered and the solvent was removed under vacuum. The residue was purified by column chromatography on silica gel.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Deping; Kuang, Daizhi; Zhang, Fuxing; Liu, Yang; Ning, Shunhua; Tetrahedron Letters; vol. 55; 51; (2014); p. 7121 – 7123;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 4028-63-1,Some common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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.

The cuprous iodide (24 mg, 0.12mmol) and tetrakis(triphenylphosphine)palladium (43 mg, 0.06 mmol) were loadedinto a Teflon-sealed flask. 2-iodo-1,3,5-trimethylbenzene (0.51 g, 2.08 mmol) andphenylacetylene (0.26 g, 2.5 mmol) were loaded into a separate flask and dissolved intriethylamine (40 mL). This solution was then cannula-transferred into the flaskcontaining the catalysts, the solution was briefly degassed under vacuum, and theflask was sealed. The mixture was stirred under nitrogen at 80 ¡ãC for 6 h. The crudeproduct was purified by column chromatography (SiO2, eluent: petroleum ether) togive 2g as a colorless liquid in 92.0percent yield. (0.42 g, 1.91 mmol). 1H NMR (300 MHz,CDCl3): 7.51-7.54 (m, 2H), 7.33 (d, J = 7.1 Hz, 3H), 6.88 (s, 2H), 2.47 (s, 6H), 2.28(s, 3H)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,4,6-Trimethyliodobenzene, its application will become more common.

Reference:
Article; An, Wenbo; Li, Gaoqiang; Ma, Jun; Tian, Youping; Xu, Feng; Synlett; vol. 25; 11; (2014); p. 1585 – 1590;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com