Author: Jessica.F

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. 202865-85-8, name is 1-Bromo-4-iodo-2-methylbenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 202865-85-8

Carbazole (1.67 g, 10 mmol), 2-bromo-5-iodobenzene (1.57 ml, 2.07 g/mL, 11 mmol), cuprous iodide(0.38 g, 0.2 mmol) and sodium tert-butoxide (1.92 g, 20 mmol) were 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, 2 ml of 1,2-diaminocyclohexane is injected (withAfter the injection, the reaction was refluxed at 110 C for 6 h, extracted, concentrated, and powdered, and purified by column chromatography to obtain a white solid product 2 in a yield of 70%.

The synthetic route of 202865-85-8 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 61272-76-2, 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. 61272-76-2 name is 4-Fluoro-2-iodoaniline, 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.

N-(4-Fluoro-2-iodophenyl)acetamide (Ian-08) A solution of acetyl chloride (2.55 g, 25.2 mmol) in anhydrous dichloromethane (10 ml) was added at 0° C. to a solution of 4-fluoro-2-iodoaniline (Ian-04) (5.93 g, 25 mmol) and triethylamine (3.5 ml) in anhydrous dichloromethane (10 ml). The mixture was stirred for 1 h at 0° C. and then overnight at room temperature and then made alkaline with 25percent potassium carbonate solution. The phases were separated and the aqueous phase was extracted with dichloromethane (2*30 ml). The combined organic phases were dried with sodium sulfate and concentrated to small volume under vacuum. The residue (7.01 g) was taken up in tetrahydrofuran (120 ml) and filtered. The filtrate was concentrated to small volume under vacuum. Yield: 6.60 g (95percent), white solid Melting point: 142-144° C. 1H-NMR (DMSO-d6): 2.03 (s, 3H); 7.25 (dt, 1H, J=8.6, 2.9 Hz); 7.37 (dd, 1H, J=8.8, 5.7 Hz); 7.75 (dd, 1H, J=8.2, 2.9 Hz); 9.46 (s, 1H).

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

Reference:
Patent; GRUNENTHAL GMBH; US2009/215725; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 4387-36-4, name is 2-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 4387-36-4, COA of Formula: C7H4IN

Preparation 1; 4′-Bromo-biphenyl-2-carbonitrile Combine 2-iodobenzonitrile (9. 0g, 38.5 mmol), 4-bromophenylboronic acid (10.4g, 51.8 mmol), 2M aqueous sodium carbonate (20 mL) and tetrakis (triphenylphosphine)- palladium (O) (4. 5g, 3.9 mmol) in 300 mL of dioxane and heat to 80°C under nitrogen with stirring. After 3 hours cool to room temperature and dilute with 900 mL of ethyl acetate. Wash with water (2 x 50mL), brine (1 x 50mL) and dry over sodium sulfate. Filter and evaporate to a yellow solid. Chromatograph on silica gel two times, eluting with a gradient of 100percent toluene to 1/9 ethyl acetate/toluene to give the title compound as a tan solid, 5.42 g (55percent). MS (FAB) = 257 (M) ; HPLC analysis is 95percent.

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

Reference:
Patent; ELI LILLY AND COMPANY; WO2005/70916; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 3718-88-5, 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. 3718-88-5, name is 3-Iodobenzylamine hydrochloride belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A suspension of 3-iodobenzylamine hydrochloride (4.95 g, 18.4 mrnol) in dichloromethane (100 mL) was treated with trieihylamine (3.1 mL, 22 mmol) and di-tert-butyl dicarbonate (4.40 g, 20 mmol) artid the resulting solution stirred at room temperature for 1.5 hours. The reaction fixture was then washed with 2M hydrochloric acid (30 mL), water (30 mL), cried over sodium sulfate and concentrated in vacuo to afford the title compound as a colourless solid in quantitative yield, 6.43 g. HNMR (400MHz, CDCI3) 8 : 1.46 (9H, s), 4.21-4. SO (2H, m), 4. 79-4. 89 (1 H, bs), 7.06 (1H, dd), 7.25 (1H, d), 7.60 (1H, d), 7.63 (1H, s); LRMS ESl m/z 332 [M-H]-

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

Reference:
Patent; PFIZER LIMITED; PFIZER INC.; WO2005/92840; (2005); 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. 170112-66-0, name is 3,4,5-Trifluoroiodobenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 170112-66-0

Set up a reflux reaction device and put a stirrer into the reaction bottle. 4-propylbiphenylacetylene, 1,2,6-trifluoro-4-iodobenzene, Catalyst Pd(Pph3)4 and cuprous iodide; Replace the air in the sealing system with argon; inject triethylamine, Tetrahydrofuran, stir and slowly heat to reflux. Make sure the system reacts under argon protection. After 7 hours, the degree of reaction was measured by TLC. Step 2), purify the crude product of step 1) with a cable extractor: After the reaction is completed, the reaction solution is poured into ice water, and dilute hydrochloric acid is added dropwise and stirred. Drip into weakly alkaline; extract the above liquid with dichloromethane, collect the organic phase, The organic phase is washed twice with brine and then dried over anhydrous sodium sulfate or anhydrous magnesium sulfate Dry, finally, rotary evaporation of the dry organic phase to give a brown solid. At this time, the brown solid is the crude product of the sonoshihira reaction. Contains target products, self-coupling by-products, and other by-products. Set up the extraction device and pour it in the extraction bottle of the Soxhlet extractor. Into petroleum ether; the brown solid is placed in a filter paper tube, Place the filter paper tube in the extraction tube of the Soxhlet extractor; Heat and reflux for 1-2 hours, and cool the petroleum ether of the extraction bottle to room temperature or lower. The product solid precipitated and was filtered using a suction device. A product having a purity of 95% or more is obtained.

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 170112-66-0.

Reference:
Patent; Shenzhen Chao Duowei Technology Co., Ltd.; Zhang Guoxian; Bao Rui; (18 pag.)CN106398714; (2018); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 260355-20-2, These common heterocyclic compound, 260355-20-2, name is 1-Chloro-4-iodo-2-(trifluoromethyl)benzene, 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.

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, stirred for 20 minutes, and the organic phase was dried over anhydrous sodium sulfate.Concentration and flash column chromatography gave 2.2 g of yellow N-(4-chloro-3-trifluoromethylphenyl)-isoxazole-4-amine powder, yield 84%.

The synthetic route of 260355-20-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhang Ruwei; Ge Baoyin; Jing Fan; Zhai Xuexu; (9 pag.)CN108633899; (2018); A;,
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 25245-27-6 as follows. Computed Properties of C8H9IO2

In a dry two necked flask were introduced N-{2-[1-(3,5-dimethoxyphenyl)-cyclohexa-2,5-dienyl]-ethyl}-4-methyl-benzenesulfonamide 3b (66 mg, 0.168 mmol), silvercarbonate (93 mg, 0.336 mmol), triphenylphosphine (6.6 mg, 0.025 mmol), 3,5-dimethoxyiodobenzene4b (89 mg, 0.336), palladium acetate (1.9 mg, 0.008 mmol) and acetonitrile (8.5mL). The mixture was warmed to 85C and stirred for 20 hours. The mixture was filteredthrough celite, which was then washed with ethyl acetate. Evaporation of the solvents led to apaste, which was purified through silica gel chromatography (Petroleum ether/EtOAc 80:20),affording 5b as a viscous oil (48 mg, 52%). IR (film, KBr, numax, cm-1): 2937, 1594, 1458, 1425,1325, 1204, 1155, 1064, 839, 732. 1H NMR (300 MHz, CDCl3): deltaH 1.38-1.50 (1H, m,CHaHxCH2N), 1.72-1.84 (2H, m, CHaHxCH2N and CH cyclopropane), 2.21-2.26 (1H, m, CHcyclopropane), 2.41 (3H, s, CH3 tosyl), 2.91 (2H, qa, 3JHH 7.3 Hz, CH2N), 3.28 (1H, broad s, CHcyclopropane), 3.77 (12H, 2OCH3 x 2), 4.46 (1H, broad s, NH), 5.20 (1H, d, 3JHH 5.3 Hz, CHolefinic), 5.82-5.84 (1H, m, CH olefinic), 6.22 (2H, s, 2CH aromatic) 6.32 (4H, s, 2CH x 2aromatic), 7.25 (2H, d, 3JHH 8.3 Hz, CH x 2 tosyl), 7.63 (2H, d, 3JHH 8.3 Hz, CH x 2 tosyl). 13CNMR (75.5 MHz, CDCl3): deltaC 21.6 (CH3 tosyl), 37.1, 38.0 (2CH cyclopropane), 38.1 (C,aliphatic), 41.2, 41.3 (2CH2, CH2CH2N), 51.2 (CH allylic), 55.4, 55.5 (2OCH3 x 2), 98.2, 98.5(2CH aromatic), 105.9, 110.0 (2CH x 2 aromatic), 127.1, 129.8 (2CH x 2 tosyl), 131.6, 134.2(2CH olefinic), 137.0, 140.0, 143.4, 146.7 (4C aromatic), 160.5, 161.0 (2C x 2 aromatic).MS(ESI) m/z (%): 1121 (2M+Na, 22), 588 (M+K, 13), 572 (M+Na, 100). HRMS calcd for[M+Na]+ C31H35NNaO6S: 572.2083; found 572.2082 (0 ppm).

According to the analysis of related databases, 25245-27-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Lebeuf, Raphael; Robert, Frederic; Landais, Yannick; ARKIVOC; vol. 2014; 3; (2013); p. 6 – 17;,
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 202982-67-0 as follows. name: 4-Chloro-3-fluoroiodobenzene

Tris(dibenzylideneacetone)dipalladium(0) (47.6 mg, 0.05 mmol), 2- (dicyclohexylphosphino)-2′,4′,6′-triisopropylbiphenyl (XPhos, 49.6 mg, 0.10 mmol), 4-chloro-3- fluoroiodobenzene (400 mg, 1.56 mmol, Aldrich), teri-butyl 2,6-diazaspiro[3.3]heptane-2- carboxylate, oxalic acid (300 mg, 1.04 mmol, ArkPharm), and cesium carbonate (1017 mg, 3.12 mmol) were suspended in dioxane (12 mL). The reaction mixture was stirred at 98 C for 18 hours and then cooled to ambient temperature. The crude reaction mixture was combined with 5 grams of Celite and concentrated under reduced pressure to a free flowing powder. The powder was directly purified by reversed-phase flash chromatography [Interchim PuriFlash C18XS 30 mupiiota 175 g column, flow rate 100 mL/minute, 5-100% gradient of acetonitrile in buffer (0.025 M aqueous ammonium bicarbonate, adjusted to pH 10 with ammonium hydroxide)] to give the title compound (0.27 g, 0.83 mmol, 79 % yield).JH NMR (400 MHz, DMSO-de) delta ppm 7.29 (t, J = 8.6 Hz, 1H), 6.42 (dd, J = 11.7, 2.6 Hz, 1H), 6.25 (ddd, J = 8.8, 2.6, 0.8 Hz, 1H), 4.01 (s, 4H), 3.94 (s, 4H), 1.38 (s, 9H); MS (ESI+) m/z 327 (M+H)+.

According to the analysis of related databases, 202982-67-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CALICO LIFE SCIENCES LLC; ABBVIE INC.; MARTIN, Kathleen Ann; SIDRAUSKI, Carmela; FROST, Jennifer M.; TONG, Yunsong; XU, Xiangdong; SHI, Lei; XIONG, Zhaoming; (165 pag.)WO2019/90090; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 19099-54-8, name is 1-Iodo-2-isopropylbenzene, molecular formula is C9H11I, 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

Specific operation: In a 25 mL reaction flask equipped with a magnetic stirrer, a metal catalyst palladium acetate (6.7 mg, 0.03 mmol), triphenylphosphine (20.0 mg, 0.075 mmol,) was added,S-2-bromophenyl-S-methyliminosulfanone (70.0 mg, 0.3 mmol), norbornene (56.4 mg, 0.6 mmol), potassium carbonate (82.8 mg, 0.6 mmol), nitrogen protection (at least three times nitrogen cycle)Acetonitrile (3 ml) and 2-iodoisopropylbenzene (88.6 mg, 0.36 mmol) were successively added under a stream of nitrogen.Closed container.The reaction was heated to 80 C for about 24 h, and the reaction was complete by TLC. After the first treatment, the reaction solution was diluted with 15 ml of ethyl acetate.Then, the catalyst and alkali and other inorganic substances are removed by suction filtration through a sand funnel containing silica gel.The resulting filtrate was separated by flash column chromatography to give the pure product 7-isopropyl-5-methyldibenzo[c,e][1,2]thiazine-5-oxide compound 3c.Yield: 40%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 19099-54-8, its application will become more common.

Reference:
Patent; Jiangxi Normal University; Chen Zhiyuan; Zhou Hao; Wang Xiumei; (17 pag.)CN107987034; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 628-77-3, name is 1,5-Diiodopentane, 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 628-77-3, Recommanded Product: 628-77-3

Preparation of Intermediate methyl 1-(4-bromoDhenyl)cvclohexanecarboxylate (1AE-1); Sodium hydride (12 g, 52 mmol) was suspended in tetrahydrofuran (200 mL) under argon and warmed to 35C. Methyl 2-(4-bromophenyl)acetate (26mmol) in tetrahydrofuran added drop wise to reaction over 1 hour. The reaction mixture was then kept at this temperature for 1 hour until all gas evolution has ceased. The 1 ,5- diiodopentane (17 g, 52 mmol) was then added drop wise as a solution in tetrahydrofuran (100 mL) and the reaction mixture stirred at 35C for a further hour and at ambient temperature overnight. After this time, the reaction mixture was cooled to 00C and quenched by the addition of dry silica, filtered and the solvent removed under vacuum. The crude product was then purified by flash chromatography eluting with 33% ethyl acetate in heptane to give methyl 1-(4-bromophenyl)cyclohexanecarboxylate (1AC-1 ) (15.3 g, 99 % yield) as a yellow oil.1 H NMR (400 MHz, CDCI3): 7.45-7.38 (m, 2 H), 7.27-7.24 (m, 2 H), 3.63 (s, 3 H), 2.43 (d, J = 13.3 Hz, 2 H), 1.71-0.80 (m, 8 H) ppm.

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; PFIZER INC.; ASPNES, Gary, Erik; DOW, Robert, Lee; MUNCHHOF, Michael, John; WO2010/86820; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com