Month: April 2021

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. 620621-48-9, name is Methyl 2-chloro-5-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: Methyl 2-chloro-5-iodobenzoate

General procedure: This compound was prepared using a method analogousto that of Example 8 (intermediate 8.1), 2-methyl-2Hpyrazol-3-ylamine replacing 4-aminopyrimidine except thatthe reaction mixture was stirred for 2 days at 80 C. LC-MS (B): tR=0.64 min; [M+H]+: 266.02

According to the analysis of related databases, 620621-48-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Actelion Pharmaceuticals Ltd.; Hilpert, Kurt; Hubler, Francis; Murphy, Mark; Renneberg, Dorte; US2014/73651; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 13421-00-6, 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 13421-00-6 as follows.

General procedure: A mixture of benzonitrile(2.0 mmol) and o-iodobenzoic acid (2.0 mmol) and [bmIm]OH (35mol) was stirred at room temperature for (3-5) h. After completion of reaction as indicated byTLC, 20mL of water was added to the reaction mixture and stirred well. The product was extracted with ether (3¡Á20 mL). The combined organic layers were dried over anhydrous Na2SO4 to afford the crude product, this crude product was taken to column in order to obtain analytically pure compound 4(a-m)(77-91%). After isolation of the product, the remaining aqueous layer containing the ionic liquid was washed with ether (2x10mL) to remove organic impurity and filtered. The filtrate was extracted with dichloromethane(2¡Á10mL), dried over MgSO4 and evaporated under reduced pressure to afford [bmIm]OH, which was reused five times in subsequent runs without further purification.

According to the analysis of related databases, 13421-00-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Waseem, Malik Abdul; Shireen; Srivastava, Anjali; Srivastava, Arjita; Rahila; Siddiqui; Tetrahedron Letters; vol. 55; 44; (2014); p. 6072 – 6076;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 622-50-4,Some common heterocyclic compound, 622-50-4, name is N-(4-Iodophenyl)acetamide, molecular formula is C8H8INO, 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, copper hydroxide (20 mol%, 2.5 mg) and a magnetite were added to a previously baked 10 mL glass pressure tube. Then, N,N-dimethylformamide (0.5 mL), 4-iodoacetanilide (0.125 mmol, 1.0 equiv., 32.6 mg) and phenylsilane (3.0 equiv., 40.6 mg) were added. The pressure tube was sealed and the tube air was removed and charged with carbon dioxide (5.0 equiv., 15 mL) and ammonia gas (0.67 mmol, 5.0 equiv., 15 mL). After the addition, the glass pressure tube was placed in a metal module that had been preheated to 160C and stirred for 10 hours. After the reaction was completed, the reaction system was cooled to room temperature and the pressure was slowly released. Using dodecane as an internal standard, the yield of the gas chromatograph was 97%.

The synthetic route of 622-50-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese Academy Of Sciences Lanzhou Chemical Physics Institute Suzhou Institute; Li Yuehui; Wang Hua; Dong Yanan; Ke Lisitian¡¤shanduofu; (20 pag.)CN108017557; (2018); A;,
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

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

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

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

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

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

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