Category: iodides-buliding-blocks

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. 64248-58-4, name is 1,2-Difluoro-4-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., 64248-58-4

General procedure: A Schlenk flask equipped with asepta and a magnetic stir bar wasfilled with aryl halide (3.0 mmol), alkene (3.2 mmol), K2CO3(3.5 mmol) and PdLn-beta-CD 3 mol% catalyst in water (5 mL pure orplain). The reaction was refluxed for the appropriate time underaerobic conditions. After completion of the reaction was confirmedby TLC, the reaction mixturewas cooled to room temperature.The solvent was removed by rotary evaporator and extraction of theproduct was carried out using ethyl acetate. The ethyl acetate fractionwas separated and dried over anhydrous sodium sulphate. Theresulting crude product was purified using flash column chromatographyof silica gel 60-120mesh with n-hexane/ethyl acetate (8:2ratio) as the eluent and afforded the pure desired product. After extractionof product, catalyst was simply reprecipitated from theaqueous layer by the addition of 10 mL of acetone. The recoveredcatalyst was filtered, washed with acetone (3 ¡Á 5 mL) and dried ina vacuum at 70 C for 5 h and reused.

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:
Article; Dindulkar, Someshwar D.; Jeong, Daham; Kim, Hwanhee; Jung, Seunho; Carbohydrate Research; vol. 430; (2016); p. 85 – 94;,
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 82998-57-0 as follows. 82998-57-0

Add 1 equivalent of potassium t-butoxide to a 25 mL Schlenk reaction tube, add 2 mL of toluene under an argon atmosphere, stir for 30 min, remove the solvent, add 0.02 equivalent of anhydrous copper sulfate and 4.0 equivalent of potassium t-butoxide, and dry in vacuum for 15 minutes. 3 mL of benzonitrile and 1 mL of t-butanol were sequentially added under an argon atmosphere, 2 mmol of 3-iodo-4-methylbenzoic acid was in the reaction tube after adding polytetrafluoroethylene stopper was placed into an oil bath of the reaction 90 C for 24 h. After the reaction is completed, 4 equivalents of formic acid are added, and the solvent is removed by filtration and the residue is purified by column chromatography eluting with petroleum ether / methylene chloride / ethyl acetate (v: v: v = 5:10:1), 6-carboxy-2-phenyl-1H-indole was obtained as a white solid. The yield was 92%.

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; University of Science and Technology of China; Kang Yanbiao; Shan Xianghuan; (12 pag.)CN108863894; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 696-41-3 name is 3-Iodobenzaldehyde, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 696-41-3

To a suspension of NaH (60% dispersion in mineral oil) (120 mg, 3.0 mmol) in THF (20 mL) was added triethyl phosphonoacetate (436 muL, 2.2 mmol) dropwise. 3-iodo-benzaldehyde (465 mg, 2.0 mmol) was added after the bubbling has stopped. The reaction mixture was stirred at room temperature for 15 minutes. Solid NH 4Cl was added, followed by 1N HCl to quench the reaction. The mixture was taken up in ethyl acetate and water. The organic phase was washed with aqueous NaHCO 3, brine, dried (MgSO 4), filtered and concentrated under reduced pressure and purified by flash chromatography on silica gel with hexane/ethyl acetate (4:1) to provide the titled compound (605 mg).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Iodobenzaldehyde, and friends who are interested can also refer to it.

Reference:
Patent; Xin, Zhili; Liu, Gang; Pei, Zhonghua; Szczepankiewicz, Bruce G.; Serby, Michael D.; Zhao, Hongyu; US2004/214870; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 455-13-0, name is 4-Iodobenzotrifluoride, 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 455-13-0, 455-13-0

General procedure: A 25 mL reaction flask was charged with copper nanoparticles (0.1 mmol)Aryl diiodonium (0.5 mmol),Benzene boronic acid (1.5 mmol),Potassium phosphate (1.0 mmol),Potassium fluoride (0.5 mmol), pivalic acid (0.5 mmol) and polyethylene glycol-400 (2.0 g)And the introduction of an atmospheric carbon monoxide.The reaction mixture was reacted at 100 C until the reaction was complete and cooled to room temperature,The product was isolated by column chromatography after evaporation of the solvent under reduced pressure.

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-Iodobenzotrifluoride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nanjing Normal University; Han Wei; Cheng Laijing; Rong Qi; (9 pag.)CN103951537; (2017); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

2401-21-0, The chemical industry reduces the impact on the environment during synthesis 2401-21-0, name is 1,2-Dichloro-3-iodobenzene, I believe this compound will play a more active role in future production and life.

PREPARATION 1 A mixture of p-aminoacetophenone (20 g), pyridine (11.7 g), and iodobenzene dichloride (40 g) in tetrahydrofuran (300 ml) was stirred for 5 hours at 0¡ã C. The insoluble materials were filtered, and the filtrate was concentrated under reduced pressure. The residue obtained was crystallized from ethanol to give colorless crystals of 4′-amino-3′-chloroacetophenone (20.1 g). IR (Nujol): 3420, 3340, 3230, 1665, 1635, 1590 cm-1.

The chemical industry reduces the impact on the environment during synthesis 1,2-Dichloro-3-iodobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Fujisawa Pharmaceutical Co., Ltd.; US4866091; (1989); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

52548-14-8, The chemical industry reduces the impact on the environment during synthesis 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of 5-methyl-2-iodobenzoic acid (3.0 g, 11 .4 mmol) in toluene (150 mL), SOCl2 (8.35 mL, 114 mmol) was added and the mixture was heated at 100C for 3 hours. Thesolvent was concentrated in vacuum and the residue was co-evaporated from toluene twice to give the title compound as a grey solid. Yield (3.2 g, 100%). 1H NMR (400 MHz, CDCl3): 6 2.42 (s, 3H), 7.09 (dd, 1 H), 7.90 (d, 1 H), 7.92 (d, 1 H).

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

Reference:
Patent; ROTTAPHARM SPA; STASI, Luigi Piero; ROVATI, Lucio; WO2013/139730; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

39998-81-7, 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. 39998-81-7, name is 2-Fluoro-4-iodo-1-methylbenzene, A new synthetic method of this compound is introduced below.

Methyl-2-fluoro-4-iodo benzoate (Reagent G) A solution of 2-fluoro-4-iodo toluene (5 g, 26.6 mmol) in pyridine (2 mL) and water (20 mL) was treated with potassium permanganate (16.6 g, 105 mmol) and heated at 150 C. overnight. The reaction mixture was then cooled to room temperature and filtered and the filtrate was extracted with hexane. The aqueous phase was acidified with 10% hydrochloric acid and extracted with ethyl acetate. The organic phase was dried over anhydrous sodium sulfate, filtered and evaporated in vacuo. The residue was dissolved in 20 mL of methanol, treated with concentrated sulfuric acid (1 mL) and refluxed overnight. The volatiles were distilled off in vacuo and the residue was dissolved in diethyl ether, washed with brine, dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to an oil. Flash column chromatography over silica gel (230-400 mesh) using 10% ethyl acetate in hexane as the eluent afforded the title compound as an oil (0.26 g, 5%). 1H NMR (300 MHz, CDCl3):delta 7.60 (m, 4H), 3.93 (s, 3H).

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; Allergan Sales, Inc.; US6252090; (2001); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

116632-39-4, The chemical industry reduces the impact on the environment during synthesis 116632-39-4, name is 5-Bromo-2-iodotoluene, I believe this compound will play a more active role in future production and life.

A Schienk tube was charged with compound 480 (402 mg, 1.31 MMOL) in 1,4-dioxane (3.0 mL), 5-BROMO-1-IODO-TOLUENE (358 mg, 1.19 MMOL), sodium tert-butoxide (160 mg, 1.67 MMOL), PD2 (dba) 3 (27 mg, 0.03 MMOL), and rac-BINAP (28 mg, 0.045 MMOL). The tube was capped with a rubber septum, flushed with argon for 5 min, and then stirred at 100 C for 72 h. The reaction mixture was allowed to cool to RT, and then poured into a mixture of water and EtOAc. The aqueous phase was extracted twice with more EtOAc. The combined organic phases were washed with brine, dried (MGSO4), filtered and concentrated in vacuo. The crude product was purified by chromatography eluting with petroleum ether/EtOAc 4: 1 to afford the title compound as yellow oil. 13C NMR (CI3) 8 195.4, 160.6, 147.7, 141.9, 137.7, 134.3, 134.0, 133.9, 133.4, 132.6, 131.6, 130.3, 130.0, 124.5, 117.6, 117.6, 116.1, 112.9, 111.0, 81.7, 67.0, 21.3, 17.8

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

Reference:
Patent; LEO PHARMA A/S; WO2005/9940; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

64248-58-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 64248-58-4 name is 1,2-Difluoro-4-iodobenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

3,4-difluoro-iodobenzene (100mg, 0.41mmoL) and piperazine (32mg, 0.41mmoL) were mixed in 5mL of dioxane, under a nitrogen atmosphere, followed by triethylamine (54mg, 0.45mmoL), 2.5 mg of X-phos (2- dicyclohexyl-P-2 ‘, 4′, 6’-triisopropyl biphenyl) and 2.5mg of Pd2 (dba) 3 (tris (dibenzylideneacetone) dipalladium) , then stirred at room temperature for 3 hours. Then vacuum to spin dioxane was added 20mL of water and 20mL of ethyl acetate, the organic phase was dried over sodium sulfate, spin dry and separate living give 37mg of product. The above product (37mg, 0.19mmoL) and piperazine (40mg, 0.55mmol), potassium carbonate (60mg, 0.43 mmol) were mixed in N, N- dimethylacetamide in a microwave at 150 stirred for 2 hours, and then spin to N, N- dimethylacetamide, purified by column to give (3-fluoro-4- (piperazin-1-yl) phenyl) dimethyl phosphine oxide (40mg).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,2-Difluoro-4-iodobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Shanghai Hansoh BioMedical Co., Ltd.; Jiangsu Hansoh Pharmaceutical Group Co., Ltd.; Yang, Fei; Zhang, Xiuchun; Sun, Xingyi; Wei, Mingsong; Wang, Chunjuan; Tong, Chaolong; Li, Chenghai; Bao, Rudi; Yu, Hongping; Xu, Yaochang; (52 pag.)CN105712928; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

101335-11-9, 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. 101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 2-chloro-4-fluoro-l-iodobenzene (10.0 g, 39.0 mmol) in dry THF (150 niL) was added /-PrMgCl (29.3 niL, 2.0 N, 58.5 mmol) dropwise at 0 C . After stirring for 1 hr at 0 C , the reaction was warmed to room temperature and stirred for 2 h. 1,4-cyclohexanedione monoethylene acetal (4.87 g, 31.2 mmol) was added and the reaction was stirred at room temperature for 12 h. Water (100 mL) was added and the mixture was extracted with ethyl acetate (3 x 100 mL). The combined organic phases were washed with brine (100 mL), then dried over Na2SO4. After concentration in vacuo, the crude material was purified by column chromatography (petroleum ethe?ethyl acetate = 5:1) on silica gel to give the desired product as a white solid (5.38 g, 48%). 1H NMR (400 MHz, CDCl3): delta 7.61-7.57 (m, IH), 7.14-7.11 (m, IH), 6.99- 6.94 (m, IH), 4.00-3.95 (m, AzU), 2.63-2.57 (m, IH), 2.42-2.36 (m, 2H), 2.17-2.10 (m, 2H), 2.05-2.01 (m, 2H), 1.72-1.69 (m, 2H).

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; SEPRACOR INC.; BURDI, Douglas; SPEAR, Kerry, L.; HARDY, Larry, Wendell; WO2010/114971; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com