Iodides-buliding-blocks

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. Recommanded Product: 116632-39-4

To a solution of 4-bromo-1-iodo-2-methylbenzene (0.24 mL, 1.6 mmol) in tetrahydrofuran (5 mL) at -78 C. was added n-butyl lithium (2.5 M in hexane, 0.8 mL, 2.0 mmol) dropwise over 15 minutes. The reaction mixture was stirred at -78 C. for 30 minutes, treated with neat cyclobutanone (0.12 mL, 1.6 mmol) dropwise over 10 minutes and stirred at -78 C. for an additional 1.5 hours. The reaction was quenched with saturated aqueous ammonium chloride solution, warmed to room temperature and extracted with ethyl acetate (2*). The combined organic layers were dried over magnesium sulfate, filtered and concentrated in vacuo to afford 500 mg yellow semi-solid, which was purified by flash chromatography (12 g silica, 0-50% ethyl acetate/heptane, 18 column volumes). Product fractions were combined and concentrated in vacuo to afford the title compound as a colorless waxy solid (290 mg, 73% yield). GCMS 240/242 (M)+; 1H NMR (400 MHz, CDCl3) delta 7.23-7.31 (m, 2H), 7.11 (d, J=8.20 Hz, 1H), 2.55-2.64 (m, 2H), 2.28-2.38 (m, 5H), 2.07-2.20 (m, 1H), 1.93 (s, 1H), 1.62-1.74 (m, 1H).

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

Reference:
Patent; PFIZER INC.; Bhattacharya, Samit; Cameron, Kimberly; Dowling, Matthew; Fernando, Dilinie; Ebner, David; Filipski, Kevin; Kung, Daniel; Lee, Esther; Smith, Aaron; Tu, Meihua; US2013/267493; (2013); A1;,
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These common heterocyclic compound, 160976-02-3, name is 5-Bromo-1,3-difluoro-2-iodobenzene, 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 C6H2BrF2I

In a nitrogen atmosphere, add 2.6-difluoro-p-bromoiodobenzene (0.32 g, 1.01 mmol),o-iodophenol (0.88g, 4.00mmol) and potassium carbonate (0.552mg, 4.00mmol),Then 15 mL of NMP (N-methylpyrrolidone) was added, and the reaction was carried out at 135 C for 12 hours;After the reaction was completed, it was filtered and washed three times with petroleum ether. The organic solutions were combined and concentrated;The crude product was purified with a silica gel column, the eluent was petroleum ether, and the final product was 0.31 g of a white solid with a yield of 43%;

The synthetic route of 5-Bromo-1,3-difluoro-2-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Xi’an Jiaotong University; Zhou Guijiang; Song Dongdong; Yang Xiaolong; Zhang Yindi; (21 pag.)CN110818738; (2020); A;,
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Electric Literature of 672293-33-3, These common heterocyclic compound, 672293-33-3, name is Methyl 4-amino-5-iodo-2-methylbenzoate, 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 NaNO2 (5.33 g, 77.25 mmol) in water (150 mL) was added dropwise to a solution of 18A (15.0 g, 51.53 mmol) in conc. HCl (150 mL) at -5 C. over a period of 20 min. The reaction mixture was stirred at -5 C. for 1 hour, then a solution of CuCl (7.72 g, 0.078 mmol) in conc. HCl (150 mL) was added. The reaction mixture was stirred at 60 C. for 4 hours. After cooling, the resulting mixture was extracted with EtOAc (400 mL¡Á3). The combined organic fractions were washed with water and brine and dried over sodium sulfate. The solvent was concentrated under reduced pressure and the residue was purified by chromatography on silica gel (4% EtOAc in pet. ether) to provide 18B (9.69 g, 60% yield) as yellow oil: ESI m/z 311, 313.0 [M+H]+.

Statistics shows that Methyl 4-amino-5-iodo-2-methylbenzoate is playing an increasingly important role. we look forward to future research findings about 672293-33-3.

Reference:
Patent; Seal Rock Therapeutics, Inc.; BROWN, Samuel David; US2018/291002; (2018); A1;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 391211-97-5, name is 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, 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 391211-97-5, COA of Formula: C13H7F3INO2

Palladium hydroxide (100 mg) was suspended in a solution of l-(diphenylmethyl)-3-(2-hydroxyethyl)azetidin-3-ol (228 mg, 0.80 mmol) in methanol (15 mL), and the mixture was subjected to an atmosphere of hydrogen at 50 psi for 4 h. The catalyst was then removed by filtration through celite, and the filtrate was concentrated in vacuo to provide 3-(2-hydroxyethyl)azetidin-3-ol. This material was used in the subsequent reaction without purification. To a solution of 3,4- difluoro-2-[(2-fluoro-4-iodophenyl)amino]benzoic acid (314 mg, 0.80 mmol), prepared using procedures similar to those described in US 7,019,033, in DMF (4 mL) was added PyBOP (416 mg, 0.80 mmol) and triethylamine (223 muL, 1.6 mmol). Finally, the unpurified 3-(2-hydroxyethyl)azetidin-3-ol was added, and the resulting mixture was stirred at rt for 16 h. Water and ethyl acetate were added, and the layers were separated. The aqueous phase was extracted with once more with ethyl acetate. The combined organic extracts were washed with brine, dried over magnesium sulfate, filtered, and concentrated in vacuo. The residue was purified by flash chromatography, eluting with ethyl acetate, to provide l-({3,4-difluoro-2-[(2-fluoro- 4-iodophenyl)amino]phenyl}carbonyl)-3-(2-hydroxyethyl)azetidin-3-ol as a colorless oil (303 mg, 0.62 mmol, 78% yield). 1H NMR (400 MHz, CDCl3): delta 8.46 (s, IH), 7.39 (dd, IH), 7.32 (m, IH), 7.13 (m, IH), 6.81 (m, IH), 6.60 (m, IH), 4.37 (br s, IH), 4.28 (br m, 4H), 3.94 (br s, 2H), 2.19 (br s, IH), 2.02 (m, 2H); MS (EI) for Ci8H16F3IN2O3: 491 (MH’).

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, 3,4-Difluoro-2-((2-fluoro-4-iodophenyl)amino)benzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; EXELIXIS, INC.; WO2008/76415; (2008); A1;,
Iodide – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 2401-21-0, name is 1,2-Dichloro-3-iodobenzene, 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 2401-21-0, Recommanded Product: 2401-21-0

EXAMPLE 35 Benzyl 3-chloro-3-ethylsulphinyl-7-oxo-1-azabicyclo[3.2.0]heptane-2beta-carboxylate STR77 A solution of benzyl 3alpha-ethylthio-7-oxo-1azabicyclo[3.2.0]heptane-2beta-carboxylate (16) (0.050 g) in methylene chloride (5 ml) was stirred in an ice bath under argon and treated with water (1 drop), pyridine (0.040 g) and iodobenzene dichloride (0.091 g). The ice-bath was removed and the reaction mixture stirred at room temperature for 3 hours. The solution was then concentrated and chromatographed on silica gel 60 (<230 mesh) eluding with ethyl, acetate/60¡ã-80¡ã petroleum ether 7:3 to give benzyl 3-chloro-3-ethylsulphinyl-7-oxo-1-azabicyclo[3.2.0]heptane-2beta-carboxylate (56) (0.037 g) as a gum; tau(CDCl3) 2.61 (5H, s, phenyl), 4.75 (2H, s, benzyl CH2), 5.55 (1H, s, C2-H), 5.6-5.9 (1H, m, C5-H), 6.5-8.0 (6H, m, C4-H2, C6 -H2, SCH2) and 8.64 (3H, t J 7 Hz, CH3). This material was unstable and had to be progressed immediately as shown in example 17. 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:
Patent; Beecham Group Limited; US4223038; (1980); A;,
Iodide – Wikipedia,
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Reference of 626-44-8, 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. 626-44-8, name is 1,3,5-Triiodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a mixture of 3-methoxy-6-(trimethylsilyl)ethynylpyridazine(0.185 g, 0.766 mmol), 1,3,5-triiodobenzene (0.100 g, 0.219 mmol), Pd2(dba)3(0.020 g, 0.021 mmol), CuI (0.004 g, 0.021 mmol), PPh3 (0.005 g, 0.021 mmol) under nitrogen atmosphere were added dry Et3N (10 mL) and toluene (10 mL). The reaction mixture was cooled to 0 C and TBAF (1 M in THF, 1.53 mL) was added dropwise and the reaction mixture was stirred for 10 min. The solution was heated to50C for 48 h. The reaction was cooled,filtered through Celiteandevaporated under reduced pressure. The crude product was purified by column chromatography on silica gel (petroleum ether/ethyl acetate2:1) to give the title compound1as a brown solid (0.055 g, 55percent).

The synthetic route of 1,3,5-Triiodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Martin, Flavia-Adina; Baudequin, Christine; Fiol-Petit, Catherine; Darabantu, Mircea; Ramondenc, Yvan; Ple?, Nelly; Tetrahedron; vol. 70; 15; (2014); p. 2546 – 2555;,
Iodide – Wikipedia,
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Reference of 696-41-3,Some common heterocyclic compound, 696-41-3, name is 3-Iodobenzaldehyde, molecular formula is C7H5IO, 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 mixture of substrate 1g (100.9 mg, 0.3 mmol), 2 (0.6 mmol), Pd(TFA)2 (10.0 mg, 10 mol%), TBHP (67.6 mg, 2.5 equiv) in DCE (2.0 mL) was charged in a glass sealed-tube and stirred under N2 atmosphere at 100 0C for 12 h. Upon completion of the reaction, saturated brine (15 mL) and dichloromethane (15 mL) were added to the mixture, then the aqueous layer was extracted with dichloromethane (15 mL ¡Á 2). The combined organic layer was dried over anhydrous MgSO4. Finally, the solution was concentrated in vacuo to provide a crude product, which was further purified via a column chromatography on silica gel (eluents: petroleum ether/ethyl acetate = 10:1) to supply the product 4.

The synthetic route of 696-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Miao-Miao; Shao, Ling-Yan; Lun, Li-Jun; Wu, Yu-Liang; Fu, Xiao-Pan; Ji, Ya-Fei; Chinese Chemical Letters; vol. 30; 3; (2019); p. 702 – 706;,
Iodide – Wikipedia,
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Reference of 19099-54-8, 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. 19099-54-8, name is 1-Iodo-2-isopropylbenzene, This compound has unique chemical properties. The synthetic route is as follows.

In a dry 25 mL Schlenk reaction tube, 74 mg of 2-isopropyl iodobenzene, 203 mg of benzoic anhydride, 71 mg of benzoxazole, 5.3 mg of palladium chloride,14 mg of tris(2-furyl)phosphine, 43 mg of copper bromide, 56 mg of norbornene, 124 mg of potassium carbonate, and 3 mL of acetonitrile.Under nitrogen atmosphere, stirring was performed at 100C for 16 hours.After the reaction was completed, the mixture was cooled to room temperature and insoluble material was removed by filtration and passed through a silica gel column (volume ratio of ethyl acetate to petroleum ether was 1:10) to obtain 136 mg of a product in a yield of 40%. The reaction process was as shown in the following formula:

The chemical industry reduces the impact on the environment during synthesis 1-Iodo-2-isopropylbenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Zhejiang University; Chen Wanzhi; Zhang Pingshun; Pan Shanfei; (24 pag.)CN107382894; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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., Application In Synthesis of 3-Iodo-4-methylbenzoic acid

INTERMEDIATE 8; [2-methyl-5-(5-methyl-1 ,3,4-oxadiaz -2-yl)phenyl]boronic acid; a) Methyl 3-iodo-4-methylbenzoate; A suspension of 3-iodo-4-methylbenzoic acid (15.00 g, 60.00 mmol) and a 4M solution of hydrochloric acid in dioxane (20.00 mL, 80.0 mmol) in methanol (20 mL) was heated in a sealed tube at 80 C with stirring. After stirring for 3 days, the mixture was cooled and ethyl acetate and saturated aqueous potassium carbonate solution were added. The organic layer was washed with brine, dried (MgS04) and evaporated in vacuo to give the title compound (15.00 g, 95%).LR S (m/z): 277 (M+1)+.

According to the analysis of related databases, 82998-57-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ALMIRALL, S.A.; AIGUADE BOSCH, Jose; CARRANCO MORUNO, Ines; WO2011/57757; (2011); A1;,
Iodide – Wikipedia,
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Application of 877264-43-2,Some common heterocyclic compound, 877264-43-2, name is (5-Fluoro-2-iodophenyl)methanol, molecular formula is C7H6FIO, 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: The product from Step B (6.2 g, 25.0 mmol) was dissolved in chloroform (170 mL) and the solution was added to a suspension of manganese (IV) oxide (43.0 g, 675 mmol) in chloroform (150 mL) and the mixture was stirred overnight at 75 C. The reaction mixture was filtered through a pad of diatomaceous earth and concentrated in vacuo to afford the desired product (3.7 g, 60% crude yield) as a yellow solid: 1H NMR (500 MHz, CDCl3) delta 10.01 (d, J=3.0 Hz, 1H), 7.92 (dd, J=8.7, 5.0 Hz, 1H), 7.60 (dd, J=8.6, 3.1 Hz, 1H), 7.10-7.06 (m, 1H).

The synthetic route of 877264-43-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Molino, Bruce F.; Liu, Shuang; Guzzo, Peter R.; Beck, James P.; US2006/52378; (2006); A1;,
Iodide – Wikipedia,
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