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. 105202-02-6, name is 2-Iodo-5-(trifluoromethyl)aniline, This compound has unique chemical properties. The synthetic route is as follows., Formula: C7H5F3IN

In a air atmosphere, 1.0 mmol of 5-carboxymethyl-2-hydroxybenzylalcohol , 1.2 mmol of 5-trifluoromethyl-2-iodoaniline,0.02 mmol p-cymene ruthenium dichloride dimer,0.03 mmol of cuprous iodide, 0.08 mmol of 1,1′-bis (diphenylphosphino) ferrocene,5.0 mmol of sodium hydroxide, and 5 ml of toluene, and then placed on a condenser tube heated to 120 C. with an oil bath with magnetic stirring for 40 hours. The oil bath was removed, 3 ml of water was added to the reaction mixture and the mixture was extracted three times with 5 ml of ethyl acetate. The organic phases were combined and dried over anhydrous magnesium sulfate for 30 minutes. The filtrate was concentrated on a rotary evaporator. The concentrated solid was extracted with methylene chloride , Recrystallized to give pure product 23, yield 81%.

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 105202-02-6.

Reference:
Patent; Luoyang Normal College; Xu Chen; Li Hongmei; Wang Zhiqiang; Lou Xinhua; Fu Weijun; (11 pag.)CN105949143; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 619-58-9, 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. 619-58-9, name is 4-Iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

In the inert gas N2 atmosphere, after dehydration and deoxidation treatment to the reaction bottle after adding 4 – iodo benzoic acid (124.0 mg, 0.5 mmol, gun for adding […] borane (290 mul, 2 mmol), reacting at room temperature 12 hours, the reaction out of the glove box, in order to have three methoxybenzene (84.09 mg, 0.5 mmol) as the internal standard, CDCl3 for dissolving, stirring 10 minutes, sampling, with nuclear magnetic resonance. Calculated 1 H and the yield is 99%. The product of nuclear magnetic data: The residue is added to the sample in 1 g silica gel, in order to 3 ml methanol as a solvent, 50 C lower reaction 3 h, the borate further hydrolysis alcohol, after the reaction, extracted with ethyl acetate three times, the combined organic layer, dried with anhydrous sodium sulfate, the solvent is removed under reduced pressure, through the silica gel (100 – 200 mesh) column chromatography purification, ethyl acetate/hexane (1:5) mixture as the eluent, to obtain the pure primary alcohol, separation and the yield is 94%.

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

Reference:
Patent; Soochow University (Suzhou); Xue Mingqiang; Xu Xiaojuan; Yan Dandan; Kang Zihan; Zhu Zhangye; Shen Qi; (9 pag.)CN109574808; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 626-44-8,Some common heterocyclic compound, 626-44-8, name is 1,3,5-Triiodobenzene, molecular formula is C6H3I3, 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.

A mixture of 3 (210.4 mg, 0.461 mmol), 4 (0.25 mL, 1.75 mmol), PdCl2(PPh3)2 (48.5 mg, 0.069 mmol), PPh3 (36.3 mg, 0.138 mmol), CuI (13.2 mg, 0.069 mmol), Et3N (2.0 mL), and THF (5.0 mL) was placed in a round-bottom flask equipped with a magnetic stirring bar. After degassing the reaction mixture several times, the reaction was carried out at 40 ¡ãC for 16 h with stirring. After the reaction mixture was cooled to room temperature, CHCl3 was added to the mixture. Precipitates were removed by filtration, and the solvent was evaporated. The residue was purified by SiO2 column chromatography (hexane as an eluent, Rf = 0.15), and crystallization was carried out to afford 5 as a colorless solid (172.5 mg, 0.373 mmol, 81percent).

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

Reference:
Article; Morisaki, Yasuhiro; Gon, Masayuki; Tsuji, Yuichi; Kajiwara, Yuichi; Chujo, Yoshiki; Tetrahedron Letters; vol. 52; 42; (2011); p. 5504 – 5507;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 135050-44-1, 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. 135050-44-1 name is 3-Chloro-4-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.

3-chloro-4-iodoaniline (15 g, 59 mmol) dissolved in diethyl [(ethyloxy)methylene]malonate (19 mL, 95 mmol) and heated at 160 C for 4 hours under a reflux condenser. The condenser was then removed and EtOH evaporated. After one hour, it was cooled to rt to solidify, broken up and the solid was suspended in hexane. The mixture was filtered and the filter cake washed with hexane several times to give a grey solid (23 g, 91%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Chloro-4-iodoaniline, and friends who are interested can also refer to it.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; BURY, MICHAEL JONATHAN; CASILLAS, LINDA N.; CHARNLEY, ADAM KENNETH; HAILE, PAMELA A.; MARQUIS JR., ROBERT W.; MEHLMANN, JOHN F.; ROMANO, JOSEPH J.; SINGHAUS, JR., ROBERT R.; WANG, GREN Z.; (153 pag.)TWI609011; (2017); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 696-41-3, 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. 696-41-3, name is 3-Iodobenzaldehyde belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

DAST (27mL, 172.41 mmol) was added to a solution of 3-lodo benzaldehyde (lOg, 43.l0mmol) in DCM (l5OmL) at 0C over a period of 10 mm. The RM was warmed to RT and stirred for 19 h.The RM was carefully quenched into ice water and extracted with DCM (2×1 5OmL).The combined organic layer waswashed with sat. NaHCO3 solution, water(lOOmL), brine(lOOmL), dried over Na2SO4 and concentrated toget crude. The crude compound was purified by CC (0-5% EtOAc in PE) to obtain 9.Og (82.5%) of 1-(difluoromethyl)-3-iodobenzene as yellow oil.

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

Reference:
Patent; GRUeNENTHAL GMBH; SCHUNK, Stefan; REICH, Melanie; JAKOB, Florian; DAMANN, Nils; HAURAND, Michael; KLESS, Achim; ROGERS, Marc; SUTTON, Kathy; WO2015/158427; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 25245-29-8, name is 5-Iodo-1,2,3-trimethoxybenzene, 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 25245-29-8, HPLC of Formula: C9H11IO3

Step 1: 2-(3,4,5-Trimethoxy-phenyl)-2,3-dihydro-furan (287) To a solution of 5-iodo-1,2,3-trimethoxybenzene (900 mg, 3.06 mmol) and 2,3-dihydrofuran (1.16 mL, 15.3 mmol) in dry DMF (8 mL) were added PPh3 (20 mg, 0.077 mmol), KOAc (901 mg, 9.18 mmol), n-Bu4NCl (850 mg, 3.06 mmol) and Pd(OAc)2 (17 mg, 0.077 mmol). The reaction mixture was stirred 18 h at 80 C. The reaction mixture was diluted with AcOEt and water. After separation, the organic layer was washed with brine, dried over anhydrous Na2SO4, filtered and concentrated. The crude residue was then purified by flash chromatography on silica gel (AcOEt/Hexane: 20/80) to afford the title compound 287 (311 mg, 1.32 mmol, 43% yield). 1H NMR: (300 MHz, CDCl3) delta (ppm): 6.59 (s, 2H), 6.45 (m, 1H), 5.45 (dd, J=10.5, 8.4 Hz, 1), 4.97 (m, 1H), 3.87 (s, 6H), 3.84 (s, 3H), 3.06 (m, 1H), 2.62 (m, 1H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Iodo-1,2,3-trimethoxybenzene, and friends who are interested can also refer to it.

Reference:
Patent; MethylGene, Inc.; US2005/288282; (2005); 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 52570-33-9 as follows. Recommanded Product: 52570-33-9

b. 3-Iodo-2-{[methoxycarbonylmethyl-(toluene-4-sulfonyl)-amino]-methyl}-benzoic acid methyl ester[0236] A mixture of 3-iodo-2-methyl-benzoic acid methyl ester (75 mmol, 20.7 g), N- bromosuccinimide (76.6 mmol, 13.8 g), benzoyl peroxide (890 mg), and CCl4 (300 mL) was refluxed with stirring for 15 h. After cooling to ambient temperature the mixture was filtered and the filtrate was concentrated in vacuo to give the title compound as a tan oil. The oil (26.3 g) was dissolved in dry DMF (75 mL). NaI (22.4 g), K2CO3 (20.5 g), and (toluene-4- sulfonylamino)-acetic acid methyl ester (19 g) were added and the mixture was stirred at ambient temperature for 24 h before it was poured into water (900 mL). The mixture was extracted with ethyl acetate (2×250 mL). The combined organic phases were washed with a solution of sodium meta-bisulfte (20 g) in water (300 mL) and water (2×300 mL) before they were dried over MgSO4 and concentrated in vacuo to give the title compound as a dark gum (38.1 g). The crude product was used in the next step without further purification; MS-(+)-ion: M+23 = 539.9.

According to the analysis of related databases, 52570-33-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; FIBROGEN, INC.; WO2007/90068; (2007); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 33348-34-4, A common heterocyclic compound, 33348-34-4, name is 4-Amino-3-iodobenzonitrile, molecular formula is C7H5IN2, 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.

INTERMEDIATE 143 – PREPARATION of 3-(2-hydroxyethyl)-2-(triethylsilyl)-1 H-indole-5- carbonitrile; 4-amino-3-iodobenzonitrile (1.65 g; 5.61 mmol), 4-(triethylsilyl)but-3-yn-1-ol (1.57 ml 7.44 mmol), Bis(diphenylphosphino)ferrocene]palladium(ll) chloride (0.276 g; 0.338 mmol), lithium chloride (0.287 g; 6.76 mmol), sodium carbonate (1.43 g; 13.52 mmol) in DMF (14 ml.) was stirred at 100 0C for 15 hours. The solution was filtered through celite, diluted in ethyl acetate, washed with brine and sodium thiosulphate, dried and concentrated under reduced pressure. The crude mixture was purified by flash chromatography on silica (eluent 2 to 20 % ethyl acetate in heptane) to yield 0.873 g (43%) of the title compound as a yellow solid. ESI/APCI(+):301 (M+H); ESI/APCI(-):299 (M-H).

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; KATHOLIEKE UNIVERSITEIT LEUVEN, K.U. LEUVEN R&;D; reMYND; GRIFFIOEN, Gerard; VAN DOOREN, Tom; ROJAS DE LA PARRA, Veronica; MARCHAND, Arnaud; ALLASIA, Sara; KILONDA, Amuri; CHALTIN, Patrick; WO2010/142801; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 444-29-1, The chemical industry reduces the impact on the environment during synthesis 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, I believe this compound will play a more active role in future production and life.

representable procedure for Suzuki reaction of 4-iodomethylbenzene and phenylboronic acid (Table 2, entry 2). The catalyst Pd(at)poly-Sty-co-diOH-Cl (5.5 mg, Pd: 0.05 mol percent), 4-iodomethylbenzene (218 mg, 1 mmol), phenylboronic acid (183 mg, 1.5 mmol), K2CO3 (276 mg, 2 mmol), and ethanol/H2O (3 ml, 2:1, v/v) were added into a 25 ml round bottomed flask, which was then heated to 70 ¡ãC for 1 h as monitored by TLC. After the reaction was finished, the catalyst was filtered and washed three times with ethyl acetate (3 ml). Then, 10 ml water was added to the filtrate, and 10 ml EtOAc was added to extract the organic compound for three times. The combined extract was evaporated to leave the crude products which were purified by column chromatography over silica gel to furnish the pure 4-methylbiphenyl as a white solid:

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, 1-Iodo-2-(trifluoromethyl)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Wang, Jiayi; Song, Gonghua; Peng, Yanqing; Tetrahedron Letters; vol. 52; 13; (2011); p. 1477 – 1480;,
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. 19718-49-1, name is Methyl 4-amino-3-iodobenzoate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: Methyl 4-amino-3-iodobenzoate

A suspension of methyl 4-amino-3-iodobenzoate (500 mg, 1.81 mmol), 1 -methyl -4-(4, 4,5,5- tetramethyl-l,3,2-dioxaborolan-2-yl)-lH-pyrazole (563 mg, 2.71 mmol), Pd(dppf)Cl2 (132 mg, 0.18 mmol) and Cs2C03 (1177 mg, 3.61 mmol) in Dioxane/H20 (10 mL/2 mL) was stirred at 90C for 8h under Nitrogen. The mixture was then diluted with H20 (30 mL) and extracted with DCM (30 mL*2). The combined organic phases were concentrated in vacuo and the residue was purified by flash chromatography on silica gel (Petroleum Ether/Ethyl Acetate = 1/1) to afford methyl 4- amino-3-(l-methyl-lH-pyrazol-4-yl)benzoate (417 mg, 100%) as a brown solid. MS Calcd.: 231, MS Found: 232 ([M+H]+).

According to the analysis of related databases, 19718-49-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; KINNATE BIOPHARMA INC.; KANOUNI, Toufike; ARNOLD, Lee D.; KALDOR, Stephen W.; MURPHY, Eric A.; TYHONAS, John; (0 pag.)WO2020/6497; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com