Month: May 2021

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. 148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, A new synthetic method of this compound is introduced below., Product Details of 148870-57-9

Based on EP 0 534 859 A solution of the (d) camphorsulphonate salt obtained in Example 4 in ethyl acetate is brought to basic pH using sodium hydroxide and then the organic phase is separated off, washed, dried over Na2SO4 and evaporated. A mixture composed of 5.6 g of potassium carbonate, 2.2 g of the above amine in 100 mL of acetone and 4 g of 3-(3-iodopropyl)-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one is then refluxed for 18 hours. The solvent is evaporated off in vacuo, and the residue is taken up in ethyl acetate and then extracted with 3N hydrochloric acid. The aqueous phase separated off is brought to basic pH using sodium hydroxide and is then extracted with ethyl acetate. After washing until neutral and drying over MgSO4, evaporation in vacuo is carried out to obtain 4.5 g of an oil which is purified on a silica column using a mixture of dichloromethane/methanol (90/10) as eluant. Yield=64%

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; LES LABORATOIRES SERVIER; CARRANZA, Maria Del Pilar; GARCIA ARANDA, Maria Isabel; GONZALEZ, Jose Lorenzo; SANCHEZ, Frederic; US2014/107334; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 112671-42-8, 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. 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows.

(1) Take 21.2 g (100 mmol) of 4-dibenzofuran boronic acid,32.6g (100mmol) of 2-iodo-5-bromonitrobenzene,(1%) Pd (PPh3) 4,40g (300mmol) sodium carbonate,Toluene (800mL), ethanol (200mL) and water (200mL),Heated to reflux, reacted for 8h, the reaction was completed;The reaction solution was extracted with ethyl acetate, and the organic phase was concentrated.A yellow solid A was obtained;

The chemical industry reduces the impact on the environment during synthesis 4-Bromo-1-iodo-2-nitrobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Yantai Xianhua Chemical Technology Co., Ltd.; Xing Qifeng; Feng Peichuan; Chen Yue; Hu Lingfeng; Chen Yili; (28 pag.)CN110698458; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 340825-13-0, name is 6-Iodo-3,4-dihydronaphthalen-1(2H)-one, 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 340825-13-0, Application In Synthesis of 6-Iodo-3,4-dihydronaphthalen-1(2H)-one

A solution of 6-iodo-3,4-dihydronaphthalen-1(2B)-one (5.0 g, 18.38 minol), 4- fluorobenzenethiol (4.11 mL, 38.6 minol) and absolute ethanol (20 mL) was cooled with an ice-water bath and bubbled with HC1 gas until saturation was reached (observed by theformation of a white precipitate). The mixture was allowed to warm to rt and stirred overnight. The mixture was dissolved in ether (250 mL) and washed sequentially with water (2 x 125 mL), 0.5 M aqueous Na2CO3 (3 xlOO mL) and brine (100 mL). The organic layer was dried and concentrated to provide a solid (9.2 g) which was a mixture of thioketal and vinyl sulfide. The solid was dissolved in chloroform (150 mL) andcooled in an ice-water bath. A solution of mCPBA (35 g, 156 minol) in DCM (200 mL)was washed with brine (50 mL), dried, filtered, and the filter cake was washed with DCM(50 mL). The combined filtrates were added dropwise in portions to the chloroformsolution of the products from above until the reaction was completed as judged by LCMS(175 ml. of the mCPBA solution was needed). The mixture was cooled in an ice bath,filtered to remove the insoluble material, and the filtrate was stirred with 10% aqueousNa2S2O3 (120 mL) for 5 min. The organic phase was separated, washed sequentially with 10% aqueous Na2S2O3 (2 x 120 mL), 10% aqueous Na2CO3 (3 x 200 mL) and brine (150 mL), dried and concentrated. The residue was purified by column chromatography on silica gel, eluting with EtOAc-hexanes (gradient from 0-20%) to give 4-((4- fluorophenyl)sulfonyl)-7-iodo-1,2-dihydronaphthalene (5.3 g, 70% yield) as a white foamy solid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 6-Iodo-3,4-dihydronaphthalen-1(2H)-one, and friends who are interested can also refer to it.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; BATT, Douglas G.; DHAR, T.G. Murali; (146 pag.)WO2018/71314; (2018); 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, Application In Synthesis of 4-Amino-3-iodobenzonitrile

2-(4,4-Dimethyl-[1,3,2]dioxaboronan-2-yl)-benzoic acid ethyl ester (19.84 g) , 2-iodo-4-cyanoaniline (18.47 g), tetrakis(triphenylphosphine) palladium (8.75 g) and potassium phosphate (35.36 g) were added to dioxane (360 ml), and the resulting mixture was heated under reflux overnight. The reaction solvent was cooled, and the produced solid was collected by filtration, washed with water and dried to thereby obtain 17.3 g (yield: quantitative) of the title compound as a yellow solid. 1H-NMR(DMSO-de) dppm: 7.47 (lH,d,J=8.5Hz), 7.6-8.0 (3H,m), 8.1-8.2 (IH,m), 8.3-8.4 (IH,m), 8.98 (IH,s), 12.05(lH,brs)

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; OTSUKA PHARMACEUTICAL CO., LTD.; WO2006/35954; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 260355-20-2, name is 1-Chloro-4-iodo-2-(trifluoromethyl)benzene, 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 260355-20-2, Recommanded Product: 1-Chloro-4-iodo-2-(trifluoromethyl)benzene

The 1-chloro-4-iodo-2-trifluoromethylbenzene (10 mmol) obtained in the reaction 1.2 was dissolved in 20 ml of toluene, and the system was sequentially added with isoxazol-4-amine (12 mmol), palladium acetate ( 0.5 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (12 mmol), 3 ml of triethylamine. After stirring for 10 minutes, add 10 ml of cesium carbonate (10 mmol). The aqueous solution was heated to 50 C for 4 hours. After the reaction was completed, 20 ml of water was added to the system, and the mixture was stirred for 20 minutes. The organic phase was dried over anhydrous sodium sulfate, concentrated, and then evaporated -(4-Chloro-3-trifluoromethylphenyl)-isoxazole-4-amine powder, yield 84%.

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; Zhang Ruwei; Ge Baoyin; Jing Fan; Zhai Xuexu; (9 pag.)CN108338175; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 4028-63-1, A common heterocyclic compound, 4028-63-1, name is 2,4,6-Trimethyliodobenzene, molecular formula is C9H11I, 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.

2,4,6-trimethyliodobenzene (12 mmol, 3 equiv), elemental selenium (12 mmol, 3 equiv), 5-methylbenzoxazole (4 mmol, 1 equiv), Cu(OAc) 2 (at room temperature) 0.4 mmol), ammonium hydrogencarbonate (12 mmol, 3 equiv) was added to the reaction tube, then filled with nitrogen, and replaced three times. Under a nitrogen reaction environment, 20 mL of DMF reaction solvent was then added, and the mixture was stirred at a reaction temperature of 140 ° C for 24 hours. After monitoring the reaction by thin layer chromatography, the reaction mixture was cooled, then diluted with ethyl acetate, and the diluted solution was transferred to a separating funnel, and extracted with saturated brine to separate the aqueous and organic phases, and then acetic acid. The aqueous phase was extracted three times with ethyl acetate. The organic phase was combined, 25 g of anhydrous sodium sulfate was added, and the mixture was allowed to stand for 30 min, and the filter cake was washed three times with 50 mL of ethyl acetate each time, then the solvent was spun off, and the product was separated by column chromatography. Deprotection: petroleum ether: diethyl ether = 98:2), yield 90percent, product weight 1.191 g.

The synthetic route of 4028-63-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wenzhou Medical University; Wu Ge; (9 pag.)CN108484518; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 3930-83-4, These common heterocyclic compound, 3930-83-4, name is 2-Iodobenzamide, 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.

General procedure: To a solution of 2-iodobenzamide (3) or 2-bromonicotinamide (6) (2.0 mmol) in DMSO (3 mL), was added aldehyde (2.2 mmol), NaN3 (260 mg, 4.0 mmol), CuBr (29 mg, 0.2 mmol), and l-proline (46 mg, 0.4 mmol). The reaction mixture was stirred at 80 C under air. After disappearance of the reactant (monitored by TLC), water (30 mL) was added to the mixture, and then extracted with ethyl acetate (15 mL) for three times. The extraction was washed with saturated NaCl solution, dried over anhydrous Na2SO4 and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using petroleum ether/ethyl acetate (10:1 to 3:1) as the eluent to give the desired products 5 or 7.

Statistics shows that 2-Iodobenzamide is playing an increasingly important role. we look forward to future research findings about 3930-83-4.

Reference:
Article; Li, Ting; Chen, Minglu; Yang, Lei; Xiong, Zhengxin; Wang, Yongwei; Li, Fei; Chen, Dongyin; Tetrahedron; vol. 72; 6; (2016); p. 868 – 874;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 618-91-7, name is Methyl 3-iodobenzoate, 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 618-91-7, Safety of Methyl 3-iodobenzoate

Dissolve methyl 3-iodobenzoate (2.0g, 7.63mmol) in THF (50mL), then add cuprous iodide (85mg, 0.44mmol) and bistriphenylphosphine palladium dichloride (150mg, 0.22mmol) ).Nitrogen was replaced three times. Under the protection of nitrogen, diethylamine (8.3 mL, 80 mmol) and trimethylsilylacetylene (1.7 mL, 12 mmol) were slowly added.Protected by nitrogen and reacted at room temperature for 24 hours.After the reaction was completed, it was filtered, and the filtrate was concentrated. Saturated brine (60 mL) was added and extracted with ethyl acetate (60 mL × 3). The organic phases were combined, dried over anhydrous sodium sulfate, filtered, and concentrated.Separation and purification by silica gel column chromatography (PE / EtOAc (v / v) = 60/1) to obtain 1 g of oily yellow liquid, yield: 78%.

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; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; Liu Bing; Bai Shun; Yang Tiping; Zhou Youbo; Zhang Yingjun; Zheng Changchun; Luo Ming; Li Shixi; Peng Dahua; Wu Shuang; Xiong Jinfeng; (203 pag.)CN107344940; (2020); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 628-77-3, name is 1,5-Diiodopentane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: iodides-buliding-blocks

Diiodopentane (1.07 mL, 7.2 mmol, 5 eq) and potassium carbonate (200 mg, 1.44 mmol, 1 eq) were added to a solution of phenol 40 (800 mg, 1 .44 mmol) in acetone (8 mL, dried over molecular sieves). The reaction mixture was then warmed to 60C and stirred for 6 hours. Acetone was removed by rotary evaporation under reduced pressure. The resulting residue was subjected to flash column chromatography (silica gel; 50/50, v/v, hexane/ethyl acetate,). Pure fractions were collected and combined and excess eluent was removed to provide 41 (800 mg, 74%). LC/MS, method 2, 4.00 min (ES+) m/z (relative intensity) 750.66 ([M+H]+, 100).

The synthetic route of 628-77-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SPIROGEN SARL; HOWARD, Philip Wilson; TIBERGHIEN, Arnaud; WO2013/53872; (2013); A1;,
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 5458-84-4 as follows. HPLC of Formula: C7H6INO3

Step 1 2-Methoxy-4-nitro-1-trifluoromethyl-benzene Following the procedure reported in JACS 2003, 125, 12502, 2-iodo-5-nitroanisole (2.79 g, 10.0 mmol), copper(I) iodide (2.2 eq, 4.19 g), and potassium fluoride (2.2 eq, 1.28 g) were dissolved in DMF. ClF2CCO2CH3 (4.4 eq, 4.7 ml) was added and the mixture was heated to 120 C. overnight. Upon cooling, the mixture was diluted with water and diethyl ether and filtered through celite. The combined organic extracts were dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The residue was purified by flash chromatography (gradient 9:1 to 1:1 Hexanes/Ethyl Acetate) to give 2-methoxy-4-nitro-1-trifluoromethyl-benzene (1.13 g, 51.1%) as a yellow oil.

According to the analysis of related databases, 5458-84-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Brotherton-Pleiss, Christine E.; Caroon, Joan Marie; Lopez-Tapia, Francisco Javier; US2010/160388; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com