Month: March 2021

Synthetic Route of 181765-86-6, 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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

2- bromo -4- chloro- 1- iodobenzene (87.5 g), 1- naphthylboronate (100 g), the tetrahydrofuran (1 L), the potassium carbonate (200.9 g) and water (720 mL) were put in 5 L three holes round bottom flask and it was stirred. The tetrakis (triphenylphosphine) palladium (0) (13.4 g) was put into the mixed solution and 80 heated for 24 hours. The reaction solution was cooled in a room temperature and it extracted in the dichloromethane. After it was dry to the magnesium sulfate it was the organic layer concentrated under reduced pressure and the solvent was removed. Material generated with the concentration were washed with the methanol and the powder I-2 of gray was obtained with 72 g.

The chemical industry reduces the impact on the environment during synthesis Methyl 5-bromo-2-iodobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Daejoo Electronic Materials Co., Ltd.; Kim, Hyung Ho; Jeon, Young Min; Nam, Sang Jin; Kim, Soo Hyun; Kim, Min Young; Kim, Jun Woo; (29 pag.)KR2016/113488; (2016); A;,
Iodide – Wikipedia,
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Electric Literature of 2043-57-4, A common heterocyclic compound, 2043-57-4, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane, molecular formula is C8H4F13I, 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.

(Y) Synthesis of 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium1,1,2,2-tetrafluoroethanesulfonate 1-Methylimidazole (4.32 g, 0.52 mol) was partially dissolved in reagent-grade toluene (50 mL) in a large round-bottomed flask and stirred vigorously. 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane (26 g, 0.053 mol) was added, and the mixture was heated under reflux at 110 C. for 24 hours. The solvent was removed under vacuum giving 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide (30.5 g) as a waxy solid.

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; Harmer, Mark Andrew; Junk, Christopher P.; US2007/100181; (2007); A1;; ; Patent; Harmer, Mark Andrew; Junk, Christopher P.; Vickery, Jemma; US2007/100184; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, 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. Product Details of 52548-14-8

1 mmol of 2-iodo-5-methylbenzoic acid, 1 mmol of formamidine hydrochloride, and 8-quinolinolato copper (B ) 0.05 mmol, 1 mmol of sodium hydroxide and 3 mL of water. Placed in the microwave reactor, the microwave reactor at 150 W power heating 100 C to 30 minutes, cooled to room temperature. The product was extracted with ethyl acetate and concentrated under reduced pressure. The product was purified by column chromatography to give a white solid in 92% yield.

The synthetic route of 2-Iodo-5-methylbenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Fujian Medical University; KE, FANG; XU, JIANHUA; LIU, CAIQIN; WU, LIXIAN; CHEN, XIAOLE; WANG, JIN; LIN, CHEN; (8 pag.)CN103864702; (2016); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 26670-89-3,Some common heterocyclic compound, 26670-89-3, name is 2-Bromo-4-iodo-1-methylbenzene, molecular formula is C7H6BrI, 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 100 mE round-bottomed flask under argon, 1 g of 2-bromo-4-iodoroluene (3.37 mmol; 1 eq) and 0.51 g methyl azetidine-3-carboxylate, hydrochloride (preparation 1; 3.36 mmol; 1 eq) were dissolved in 10 mE of toluene. The solution was degassed with argon 4.39 g of cesium carbonate (13.47 mmol; 4 eq) 62mg of Pd2(dba)3 (0.07 mmol; 0.02 eq). and 117 g of Xant-Phos (0.20 mmol; 0.06 eq) were successively added and the reaction medium was stirred at 100 C. overnight. It was brought back to RT and diluted in EtOAc, then washed with watet The aqueous phase was extracted once again with EtOAc. The combined organic phases were dried over MgSO4, filtered and evaporated to give 1.15 g of a colorless oil. It was purified by flash chromatography on silica using a cyclohexane/0% to 10% EtOAc gradient, to give 510mg of the title compound in the form of a brown oil.Yld: 53%.?H NMR (300 MHz, DMSO-d5) oeppm 2.21 (s, 3H); 3.55-3.70 (m, 1H); 3.67 (s, 3H); 3.84-3.87 (m, 2H);3.97-4.03 (m, 2H); 6.39 (dd, J=8.4, 2.4 Hz, 1H); 6.65 (d, J=2.4 Hz, 1H); 7.13 (d, J=8.4 Hz, 1H).11015] LC-MS: m/z (M+H): 284.

The synthetic route of 26670-89-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INVENTIVA; BOUBIA, Benaissa; MASSARDIER, Christine; GUILLIER, Fabrice; POUPARDIN, Olivia; TALLANDIER, Mireille; AMAUDRUT, Jerome; BONDOUX, Michel; FEENSTRA, Roelof Williem; VAN DONGEN, Maria Johana Petronella; (207 pag.)US2017/66717; (2017); 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. 52548-63-7, name is 5-Fluoro-2-iodobenzoic acid, A new synthetic method of this compound is introduced below., SDS of cas: 52548-63-7

To a solution of 5-fluoro-2-iodo- benzoic acid (3.86 g, 14.65 mmol), 2H-[1 ,2,3]triazole (2.5 g, 36.2 mmol),Cs2CO3 (8.62 g, 24.5 mmol), trans-N, N’-dimethyl-cyclohexane-1 ,2-diamine (0.4 ml_), Cul (244 mg) and DMF (13 ml_) were added to a microwave ready vessel and heated to 100 C for 10 min. The mixture was cooled, diluted with water, and extracted with EtOAc. The aqueous layer was acidified and extracted with EtOAc. The organic layer was dried over Na2SO and concentrated. The residue was purified by FCC (SiO2, gradient DCM to 10% MeOH/1 %HOAc/DCM) gave the product as a white powder, (2.14 g, 71 %). 1H NMR (400 MHz, CD3OD): 7.91 (s, 2H), 7.76 (dd, J = 8.9, 4.8 Hz, 1 H), 7.59 (dd, J = 8.5, 2.9 Hz, 1 H), 7.49 – 7.42 (m, 1 H).; Intermediate 53: 2-[1 ,2,3]Triazol-1 -yl-benzoic acid.The title compound was isolated from the synthesis of Intermediate 13. 1H NMR (400 MHz, CD3OD): 6.70 (d, J = 0.9 Hz, 1 H), 6.50 (dd, J = 7.7, 1 .5 Hz, 1 H), 6.30 (d, J = 1 .0 Hz, 1 H), 6.24.6.18 (m, 1 H), 6.17 -6.1 1 (m, 1 H), 6.01 (dd, J = 7.8, 1 .0 Hz, 1 H).

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; JANSSEN PHARMACEUTICA NV; BRANSTETTER, Bryan, James; LETAVIC, Michael, A.; LY, Kiev, S.; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.; WO2011/50200; (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. 14452-30-3, name is 1-(3-Iodophenyl)ethanone, A new synthetic method of this compound is introduced below., Safety of 1-(3-Iodophenyl)ethanone

General procedure: In a typical experiment, a predetermined amount of Ni-MOF-74 was added to the 8 mL vial containing a mixture of iodobenzene (0.1030 g, 0.5 mmol), benzothiazole (0.1379 g, 1.0 mmol), Li2CO3 or KCl (1.0 mmol), and diphenyl ether (0.085 g, 0.5 mmol) as standard. 1-Methoxy-2-(2-methoxyethoxy)ethane (diglyme) (1 mL) was added and vial was tightly capped. Reaction mixture was heated at 160C for 24 h. The catalyst loading was based on the molar ratio of nickel/iodobenzene. The reaction yield was monitored by withdrawing aliquots from the reaction mixture at different time intervals, diluting with ethylacetate (2 mL), quenching with an aqueous KOH solution (1%, 1 mL), and then drying over anhydrous Na2SO4 before analyzing by GC with reference to diphenyl ether (internal equation with pure product), and further confirming product identity by GC-MS and NMR. To investigatethe recycle ability of Ni-MOF-74, the catalyst was filtered from the reaction mixture after the experiment, washed with ethylacetate, water, THF, and dried at 140C under vacuum in 8 h. For the leaching test, a catalytic reaction was stopped after 12 h, analyzed by GC, and filtered to remove the solid catalyst. The reaction solution was then stirred for a further 12 h. Reaction progress, if any, was monitored by GC as previously described.

The synthetic route of 14452-30-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Nguyen, Huong T.T.; Doan, Duc N.A.; Truong, Thanh; Journal of Molecular Catalysis A: Chemical; vol. 426; (2017); p. 141 – 149;,
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 19094-56-5 as follows. Computed Properties of C7H4ClIO2

General procedure: To a stirred suspension of 2-chloro-5-iodobenzoic acid(5.65 g, 0.02 mol) in CH2Cl2(20 mL) was added oxalylchloride(1.80 mL, 0.021 mol) and DMF(0.02 mL). Theresulting mixture was stirred for 4 h at room temperature.The mixture was concentrated, and the residual colorlesssolid was dissolved in CH2Cl2(40 mL). To this solutionwere added corresponding substituted benzene(0.02 mol)and then AlCl3(2.75 g, 0.021 mol) portionwise so that thetemperature did not exceed 0 C. After being stirred at 10-20 C for 3 h, the mixture was poured into ice water andextracted with CH2Cl2 three times. The combined organiclayers were washed with 1M HCl, water, and brine, thendried over MgSO4 and concentrated. The residual solid wascrystallized from ethanol to give as white solid.According to this procedure the following compoundswere prepared.

According to the analysis of related databases, 19094-56-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Hu, Shengquan; Sun, Wuji; Wang, Yeming; Yan, Hong; Medicinal Chemistry Research; vol. 28; 4; (2019); p. 465 – 472;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 82998-57-0, 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

3-lodo-4-methylbenzoic acid (3.07 g, 0.0117 mol) was added thionyl chloride (10 mL) and refluxed for 2 h. The excess thionyl chloride was carefully removed and the resulting acid chloride was dried in vacuo for 2 h. The residue was then dissolved in DCM (anhydrous, 25 mL) and cooled on ice. To the cooled solution was added 3-(1H-imidazol-1-yl)-5- (trifluoromethyl)aniline 5 (3.46 g, 0.0152mol) in DCM followed by the dropwise addition of diisopropylethylamine (8.2 mL, 0.047 mol). This was stirred at ambient temperature for 21 h. The white solid that separated was filtered and washed with water and dried to provide 4.65 g of product. Additional product could be obtained from the filtrate following concentration and purification by silica gel flash chromatography in EtOAc/hexanes.

The chemical industry reduces the impact on the environment during synthesis 3-Iodo-4-methylbenzoic acid. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ARIAD PHARMACEUTICALS, INC.; WO2007/75869; (2007); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 160976-02-3, A common heterocyclic compound, 160976-02-3, name is 5-Bromo-1,3-difluoro-2-iodobenzene, molecular formula is C6H2BrF2I, 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.

Under a nitrogen atmosphere, to a three-necked flask equipped with a reflux condenser were added 2,6-difluoro-4-bromoiodobenzene (13.3g, 41.67mmol),9-methyl-9H-carbazole-4-ol (18g, 91.67mmol), potassium carbonate (23g, 166.68mmol) and 200mL N-methylpyrrolidone (NMP), and heated to reflux for 6h.After the reaction, the system was cooled to room temperature. After adding a large amount of water, a white precipitate is formed, which is collected by suction filtration. The precipitate was washed sequentially with water and methanol (50% (V / V)).Finally, the obtained filter cake was dissolved in an appropriate amount of dichloromethane and further purified by column chromatography (mobile phase: petroleum ether: dichloromethane = 3: 1 (V / V)),23g of white solid was obtained with 82% yield.

The synthetic route of 160976-02-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Suzhou Jiuxian New Materials Co., Ltd.; Cui Linsong; Liu Xiangyang; Zhang Yexin; Chen Hua; (56 pag.)CN110981899; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 160976-02-3, The chemical industry reduces the impact on the environment during synthesis 160976-02-3, name is 5-Bromo-1,3-difluoro-2-iodobenzene, I believe this compound will play a more active role in future production and life.

General procedure: A Schlenk tube was dried using heat gun under reduced pressure and filled with argon. The tube was charged with TPPO (69.5mg, 0.25mmol) and then the tube was evacuated and refilled with argon (¡Á3). To the tube were added THF (1mL), Me2Zn (0.6mL, 0.6mmol, 1.0M solution in hexane), and fluoroarene 1 (0.75mmol) at room temperature and then the tube was immersed in an oil bath. The reaction mixture was gradually warmed to 75C and stirred for 3h. The mixture was cooled to room temperature and allylic bromide (0.5mmol) was added. The resultant mixture was warmed to 75C and stirred for 16h. The reaction mixture was quenched with saturated aqNH4Cl solution followed by extraction with Et2O (¡Á3). Combined organic layer was washed with brine (¡Á1), dried over Na2SO4, and filtered. Volatiles were removed under reduced pressure and the residue was purified by flash column chromatography on silica gel to afford analytically pure 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, 5-Bromo-1,3-difluoro-2-iodobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Kurauchi, Daisuke; Hirano, Keiichi; Kato, Hisano; Saito, Tatsuo; Miyamoto, Kazunori; Uchiyama, Masanobu; Tetrahedron; vol. 71; 35; (2015); p. 5849 – 5857;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com