Category: iodides-buliding-blocks

Reference of 13194-68-8, The chemical industry reduces the impact on the environment during synthesis 13194-68-8, name is 4-Iodo-2-methylaniline, I believe this compound will play a more active role in future production and life.

To 4-iodo-2-methylaniline (23.3g) (available from Fluorochem) in ice (6Og) and concentrated hydrochloric acid (30ml) was added a solution of sodium nitrite (7.05g) in water (18ml) slowly with stirring over 20min, keeping the temperature below 50C. The mixture was allowed to stand at 0-50C for 2h, then added slowly at 0-50C over 30min to a mixture of diethyl malonate (17ml), ethanol (300ml) and water (50ml) containing sodium acetate (18.8g). The mixture was stirred for 2h at 0-50C then for 2h at 210C. The mixture was concentrated in vacuo to a volume of about 200ml, and the product was collected by filtration, washed with water (200ml) and dried under vacuum to give the title compound as a brown solid (28.9g). LC/MS Rt 3.85min m/z 405 [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, 4-Iodo-2-methylaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLAXO GROUP LIMITED; WO2007/45861; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 25309-64-2, name is 1-Ethyl-4-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. Quality Control of 1-Ethyl-4-iodobenzene

General procedure: A mixture of compound 2 (500 mg, 1.38 mmol), triethylamine (0.6 mL, 4.14 mmol), and 1-chloro-4-iodobenzene (1.55 mmol) in DMF (3.45 mL) was treated with palladium(II) acetate (15.5 mg, 0.04 mmol) and then heated at 80 ?C under air. After 20 h, the resulting solution was allowed to cool to room temperature, water (7 mL) was added, and the resultant mixture was extracted with ether (7 mL ¡Á 5). The organics was dried over Na2SO4 and concentrated under reduced pressure to give a crude residue, which was purified by silica gel column chromatography to afford the product.

The synthetic route of 1-Ethyl-4-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ding, Ya-Hui; Fan, Hong-Xia; Long, Jing; Zhang, Quan; Chen, Yue; Bioorganic and Medicinal Chemistry Letters; vol. 23; 22; (2013); p. 6087 – 6092;,
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. 3058-39-7, name is 4-Iodobenzonitrile, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

To phenol (1.23 g, 13.10 mmol), copper(l) iodide (333 mg, 1.75 mmol), cesium carbonate (5.69 g, 17.47 mmol), 4-iodobenzonithle (2.00 g, 8.73 mmol) and N,N-dimethylglycine hydrochloride (366 mg, 2.62 mmol) under nitrogen was added degassed 1 ,4- dioxane (10.0 ml_). The whole mixture was heated at 90 0C for 88 hours. The cooled mixture was partitioned between ethyl acetate (100 ml_) and water (100 ml_). The organic layer was separated and the aqueous layer was extracted with ethyl acetate (2 x 100 ml_). The organic layers were combined and washed with brine (100 ml_) and dried with Na2SO4 and concentrated in vacuo. The crude material was purified by column chromatography EtOAc/ Hex (1 :12 ? 1 :8) to give the pure product as a white solid (quantative yield). 1H NMR (300 MHz, CDCL3) d(ppm): 7.00 (2H, d, J = 9.1 Hz), 7.06 (2H, d, J = 7.6 Hz), 7.23 (1 H, t, J = 7.2 Hz), 7.41 (2H, t, J = 8.1 Hz), 7.59 (2H, d, J = 9.1 Hz). 13C NMR (75 MHz, CDCL3) d(ppm): 105.9, 118.0 (CH), 119.0, 120.5 (CH), 125.3 (CH), 130.4 (CH), 134.2 (CH), 154.9, 161.8. MS (FAB+): 196 (MH+). HRMS for Ci3H9NO (MH+): calculated: 196.0762; found 196.0780.

The synthetic route of 3058-39-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; UNIVERSITY OF NOTRE DAME DU LAC; WO2009/41972; (2009); 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., Safety of 5-Fluoro-2-iodobenzoic acid

The 5-fluoro-2-iodo-benzoic acid by adding 13.87mol/L thionyl chloride in a solvent, heating to 60 C, stirring sleepovers Go fully clarified, TLC (PE/EA:10/1) monitoring after the reaction, to evaporate the solvent, adding toluene to dryness, ethyl acetate to dissolve the spare. 3658 g of diethyl malonate was added to 55 L of ethyl acetate, and 4762 g of magnesium chloride was added thereto at room temperature for 30 minutes. 4877 g of triethylamine was added dropwise, and the mixture was stirred for 30 minutes and cooled to 5 C. (5L X 2) was added under ice-cooling, and the organic phase was washed with saturated brine (10 L X), and the mixture was stirred at room temperature for 2 hours. TLC (PE / EA: 10/1) 2) Wash, separate and evaporate the organic layer to give a red oil. Add 12L of a mixture of acetic acid: water: concentrated sulfuric acid volume ratio of 6.6: 4.4: 1, heated to 100 C, stirred overnight (30LX 1), saturated brine (10 L X 2), dried and evaporated to dryness to give a red color. The organic phase was washed with 0.5N sodium hydroxide solution (30 LX 1) and saturated brine (10 L X 2) The product was obtained by passing the superfine silica gel column (PE / EA: 8/1)3.6Kg 1- (5-fluoro-2-iodophenyl)ethanone having the structural formula shown in Formula 3:

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; WuhanPharmaceutical Technology (Shanghai) Co., Ltd.; Guo, SongPo; Qiu, dongcheng; (9 pag.)CN105732355; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 25245-29-8,Some common heterocyclic compound, 25245-29-8, name is 5-Iodo-1,2,3-trimethoxybenzene, molecular formula is C9H11IO3, 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.

PREPARATION EXAMPLE 49 Synthesis of 2,6-dimethoxy-4-iodophenol: To a solution of 5-iodo-1,2,3-trimethoxybenzene (3.2 g) in 1,2-dichloroethane (40 mL) was added aluminum chloride (1.6 g). The mixture was stirred at 60 C. for 4 hours and evaporated. The residue was dissolved in 1 M aqueous sodium hydroxide solution and washed with ether. The aqueous layer was then acidified and extracted with chloroform. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and evaporated to give the title compound as white crystalline powder. Yield: 1.0 g (31%)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Iodo-1,2,3-trimethoxybenzene, its application will become more common.

Reference:
Patent; Kowa Co., Ltd.; US6395753; (2002); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 202865-85-8, name is 1-Bromo-4-iodo-2-methylbenzene, 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. COA of Formula: C7H6BrI

9,9-Dimethyl-9,10-dihydroacridine (2.09 g, 10 mmol), 2-bromo-5-iodobenzene (1.57 mL, 2.07 g/ml, 11 mmol), cuprous iodide ( 0.38g, 0.2mmol)Sodium tert-butoxide (1.92 g, 20 mmol) was added to the reaction flask, and nitrogen gas was exchanged three times (10 min/time), and the solvent (1,4-dioxane) was injected under a nitrogen atmosphere.After the raw material is partially dissolved, inject 2ml.1,2-diaminocyclohexane (coordinating agent),After the injection, the reaction was refluxed at 110 C for 6 h, extracted, concentrated, and powdered.Purification by column chromatography gave a white solid product 2, yield 70%.

The synthetic route of 1-Bromo-4-iodo-2-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; South China University of Technology; Tang Benzhong; Zhao Zujin; Hu Shimin; Qin Anjun; Hu Rongrong; Wang Zhiming; (24 pag.)CN109593079; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 202865-85-8, name is 1-Bromo-4-iodo-2-methylbenzene, 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

To a 2:1 (v/v) toluene: ethanol solution (0.034 M) of methyl 3-methyl-2 -(4,4,5,5- tetramethyl-l,3,2-dioxaborolan-2-yI)benzoate (1 eq.) from the previous step and 2- bromo-5-iodotoluene (1.2 eq.) was added was added trans-bis(triphenylphospliine) palladium(II) bromide (0.12 eq.). The vessel was repeatedly evacuated and back-filled with nitrogen. Finally, Na2C03 (2 M aq. solution, 3 eq.) was added and the resulting mixture was heated at 50 C for 12 h. The now black suspension was cooled to RT, diluted with ether and quenched with 10% aq. HC1. The aqueous layer was separated and back-extracted with ether. The combined organic extracts were then washed further with 1 N aq. NaOH, water and brine, dried over Na2S04, filtered and the filtrate concentrated in vacuo. Purification of the crude product by way of flash chromatography (Si02, Hex -> 1 :1 (v/v) Hex: EtOAc) afforded the title compound as a colorless oil.

The synthetic route of 1-Bromo-4-iodo-2-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK FROSST CANADA LTD.; CHEN, Austin; ASPIOTIS, Renee; MCKAY, Daniel; HAN, Yongxin; FOURNIER, Pierre-Andre; WO2011/57382; (2011); A1;,
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. 199786-58-8, name is (5-Bromo-2-iodophenyl)methanol, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C7H6BrIO

In a 1 L 3 -necked round-bottom flask (5-bromo-2-iodophenyl)methanol (14.0 g, 44.7 mmol) and IH-imidazole (6.09 g, 89.0 mmol) were combined with dichloromethane (150 mL). Then ieri-butylchlorodimethylsilane (10.1 g, 67.1 mmol) was added dropwise at 0-4C. The resulting mixture was stirred at ambient temperature for 16 hours then water (50 mL) was added. The resulting mixture was extracted with ethyl acetate (3 x 50 mL) and the combined organic layers were washed with brine (50 mL), dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo and the residue purified on silica, eluting with 5-10% ethyl acetate in petroleum ether to afford the title compound. 1H NMR (400 MHz, CDC13) 57.67- 7.62 (m, 2H), 7.15-7.12 (m, 1H), 4.61 (s, 2H), 1.01 (s, 9H), 0.20 (s, 6H).

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 199786-58-8.

Reference:
Patent; MERCK SHARP & DOHME CORP.; CHILDERS, Matthew Lloyd; DINSMORE, Christopher; FULLER, Peter; GUERIN, David; KATZ, Jason David; PU, Qinglin; SCOTT, Mark E.; THOMPSON, Christopher F.; ZHANG, Hongjun; FALCONE, Danielle; TORRES, Luis; BRUBAKER, Jason; ZENG, Hongbo; CAI, Jiaqiang; DU, Xiaoxing; WANG, Chonggang; BAI, Yunfeng; KONG, Norman; LIU, Yumei; ZHENG, Zhixiang; WO2014/146490; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 791642-68-7, 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. 791642-68-7, name is 4-Bromo-1-iodo-2-methoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 5-bromo-2-iodoanisole (533 mg, 1.30 mmol) and oxetan-3-one (0.12 mL, 2.0 mmol) in tetrahydrofuran (5 mL) at -78 C. followed by the addition of n-butyl lithium (2.5M in hexane, 0.56 mL, 1.4 mmol) dropwise over 5 minutes. The reaction mixture was stirred at -78 C. for 2 hours. The reaction mixture was quenched with saturated aqueous ammonium chloride, warmed to room temperature and extracted two times with ethyl acetate. The combined organic layers were dried over sodium sulfate, filtered, and concentrated under reduced pressure yielding 476 mg of crude material. The crude material was purified using the Biotage Isolera One (SNAP 25 g silica gel column) and eluting with a gradient of 0-70% ethyl acetate/heptane yielding 137 mg (41% yield) of the title compound. 1H NMR (500 MHz, CDCl3) delta 7.15 (dd, J=8.1, 1.7 Hz, 1H), 7.13 (d, J=8.1 Hz, 1H), 7.07 (d, J=1.5 Hz, 1H), 4.99 (d, J=7.1 Hz, 2H), 4.84 (d, J=7.3 Hz, 2H), 3.87 (s, 3H)

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, 4-Bromo-1-iodo-2-methoxybenzene, other downstream synthetic routes, hurry up and to see.

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;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 33348-34-4, name is 4-Amino-3-iodobenzonitrile, 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 33348-34-4, HPLC of Formula: C7H5IN2

General procedure: An oven-dried flask was charged with o-iodoaniline (13 mmol), the corresponding benzyl bromide(10 mmol), NaHCO3 (20 mmol), and DMF (20 mL). The mixture was stirred at 50 C under air for 3-4 h.After the completion of the reaction (monitored by TLC), the reaction mixture was cooled to ambienttemperature and 15 mL water was added to the mixture, then extracted by EtOAc for 3 times (3 ¡Á 30 mL).The combined extracts were washed with brine, dried over Na2SO4, and the solvent was removed in vacuoto provide a crude product, which was purified by column chromatography on silica gel to afford 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, 4-Amino-3-iodobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Chen, Zhengkai; Li, Hongli; Cao, Gangjian; Xu, Jianfeng; Miao, Maozhong; Ren, Hongjun; Synlett; vol. 28; 4; (2017); p. 504 – 508;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com