Iodides-buliding-blocks

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. 5460-32-2, name is 4-Iodo-1,2-dimethoxybenzene, A new synthetic method of this compound is introduced below., SDS of cas: 5460-32-2

General procedure: To a stirred solution of 4-iodoanisole (5.85 g, 25 mmol), 4-bromoaniline (1.72 g, 10 mmol), and 1,10-phenanthroline (0.18 g, 1 mmol) in toluene (100 mL) were added potassium hydroxide (5.61 g, 100 mmol) and copper(I) iodide (0.19 g, 1 mmol). The reaction mixture was heated under reflux for 24 h at 125 ¡ãC. The crude product was extracted into dichloromethane, and the organic layer was washed with 1 N HCl solution, brine, and water. The organic layer was dried with anhydrous MgSO4 and then the solvent was removed in vacuo. The residue was purified by column chromatography using silica gel and dichloromethane-hexane (1:1; v/v) as the eluent to give 3 (2.39 g, 62.2percent).

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:
Article; Kim, Se Hun; Choi, Jun; Sakong, Chun; Namgoong, Jin Woong; Lee, Woosung; Kim, Dong Hoe; Kim, Boeun; Ko, Min Jae; Kim, Jae Pil; Dyes and Pigments; vol. 113; (2015); p. 390 – 401;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 199786-58-8, 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. 199786-58-8 name is (5-Bromo-2-iodophenyl)methanol, 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.

C. N, N-DIMETHYL-5-BROMO-2-IODOPHENYLACETAMIDE 5-Bromo-2-iodobenzoic acid (100 g, 0.306 mol) is dissolved in THF (350 mL) and cooled in an ice bath. Borane-THF complex (460 mL of 1 M in THF, 0.460 mol) is added dropwise. After addition is complete, the reaction is warmed to room temp and stirred for 14 hours. The mixture is transferred a large ERLENMEYER FLASK (4 L), cooled in an ice bath and carefully quenched with water (250 mL). Evaporation of the THF by rotary evaporator gives a white suspension which is treated with additional water (1 L) and then filtered and dried in a vacuum dessicator over P205 to give 5-bromo-2-iodobenzyl alcohol. The above benzyl alcohol is dissolved in 48% HBr (500 mIL and heated at reflux temperature for 4 hours. The resulting benzyl bromide is isolated as a yellow solid by pouring the cooled mixture into a large volume (1.5 L) of water followed by filtration. The benzyl bromide is dissolved in EtOH (400 mL) and stirred at room temperature. Sodium cyanide (56 g, 1.14 mol) is dissolved in a minimum amount (-100 mL) of water and then added to the ethanolic solution of the benzyl bromide. The reaction is heated to reflux temperature for 3 hours and then cooled to room temperature. Ethanol is removed by rotary evaporator and the residue washed with a large volume (1 L) of water. The resulting 5-bromo-2-iodophenylcetonitrile is isolated by filtration. The above phenylacetonitrile is dissolved in ETOH (350 mL) and treated with NAOH (32 g, 0.8 mol) which had been dissolved in water (200 mL). The reaction is heated at reflux temperature for 14 hours. After cooling to room temperature, ethanol is removed by rotary evaporator and 6 N HCI added until the pH = 1. The solid 5-bromo-2-iodophenylacetic acid that formed is filtered and washed with water (2 x 500 mL). After drying over P205 in a vacuum dessicator, 5-BROMO-2-IODOPHENYLACETIC acid (m. p. 165-169C) (102 g, 0.3 mol) is dissolved in CH2CI2 (450 mL) that contains several drops of DMF. Thionyl chloride (32 mL, 0.450 mol) is added and the reaction heated to reflux temperature overnight. After cooling to room temperature, the reaction mixture is diluted with additional CH2CI2 (500 mL) and washed with water (2 x 250 mL), saturated NAHCO3 (250 mL) and brine (250 mL). The solution is dried (MGS04) and concentrated by rotary evaporator to give 5-bromo-2- iodophenylactetyl chloride as a yellowish oil. Dimethylamine (200 mL of 2 M in THF) is added dropwise to a solution of the above 5-bromo-2-iodophenylacetyl chloride in ET20 (500 mL), cooled in an ice bath. After the addition is complete, EtOAc (350 mL) is added and the solution washed with water (350 mL), brine (250 mL) and dried (MGS04). Evaporation by rotary evaporator and trituration with 1: 1 ET2O/HEXANES GIVES N, N-DIMETHYL-5-BROMO-2-IODOPHENYLACETAMIDE (m. p. 127-129C).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (5-Bromo-2-iodophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GMBH; WO2004/48314; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 627-32-7, 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. 627-32-7 name is 3-Iodo-1-propanol, 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.

E: 3-(4-Bromo-2-(trifluoromethyl)-phenoxy)propan-1-ol 3-Iodopropanol (11.23 g) was added to a mixture of 4-bromo-2-(trifluoromethyl)-phenol (15 g) and potassium carbonate (17.2 g) in acetonitrile (150 ml). The above mixture was refluxed for 4 hours then diluted with ethyl acetate (500 ml) and water (300 ml). Organic layer was separated, dried over magnesium sulphate, solvent removed under reduced pressure to give expected product clean enough for use at the next step (18.6 g). 1H NMR (CDCl3) delta: 7.67 (d, 1H), 7.58 (dd, 1H), 6.90 (dd, 1H), 4.18 (t, 2H), 3.87 (q, 2H), 2.07 (tt, 2H).

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

Reference:
Patent; N. V. Organon; US2009/99172; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 69113-59-3, A common heterocyclic compound, 69113-59-3, name is 3-Iodobenzonitrile, molecular formula is C7H4IN, 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: A solution of n-butyllithium inn-hexane (1.6 M, 7.4 mL, 11.9 mmol) was added to a solutionof m-carborane (1.50 g, 10.8 mmol) in l,2-dimethoxyethane(DME) (12 mL) at 0C under Ar atmosphere, and the mixture was stirred at 0 C for 30 min. Copper(I) chloride (10 mg,104 mmol) was added to the reaction mixture at room temperature. After 1 h, pyridine (3.8 mL) and substituted iodobenzene(11.9 mmol) were added, and the mixture was stirred at 80 C for 2.5 h. After cooling, the reaction mixture was diluted withether, and insoluble materials were filtered off through celite.The filtrate was washed successively with 5% sodium thiosulfate, 2 M hydrochloric acid, and brine, dried over sodiumsulfate, and evaporated. The residue was purified by silicagel column chromatography (eluent: n-hexane-ethyl acetate,20 : 1) to give 10-12.

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:
Article; Mori, Shuichi; Takagaki, Ryohei; Fujii, Shinya; Urushibara, Ko; Tanatani, Aya; Kagechika, Hiroyuki; Chemical and Pharmaceutical Bulletin; vol. 65; 11; (2017); p. 1051 – 1057;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 35453-19-1, 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. 35453-19-1, name is 5-Amino-2,4,6-triiodoisophthalic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Synthesis of 5-Amino-2,4,6-triiodo-isophthaloyl dichloride (1)5-Amino-2,4,6-triiodo-isophtalic acid (30 g, 0.054 mol) (commercially available from Aldrich), thionyl chloride (8.2 ml, 0.113 mol) and pyridine (0.2 ml) in 1 ,2 dichloroethane (20 ml) were heated to 70 0C. A portion of thionyl chloride (15.2 ml, 0.21 mol) was added dropwise during VA to 2 hrs, and the mixture was heated to 85 0C for 6 hrs. After cooling the reaction mixture to room temperature, it was poured into 30Og of ice-water. The yellow precipitate that formed was filtered off, air dried and then washed with water until washings showed a pH of ca 5. The filter cake was then dried in a vacuum oven at 5O0C for 3 hrs. A light yellow powder was obtained 31 g (~ quant.) as the desired product.13C NMR (DMSOd6) 66, 78.4, 148.9, 149.2, 169MS (ES-) found 593.5 [M-H+], expected 593.7

The synthetic route of 5-Amino-2,4,6-triiodoisophthalic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GE HEALTHCARE AS; WO2009/5365; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 69113-59-3, These common heterocyclic compound, 69113-59-3, name is 3-Iodobenzonitrile, 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: Palladium Catalyzed Heck Reaction (Conventional Heating) Sodium acetate (3 mmol), substituted piperazine (1.5 mmol), iodo-benzene or bromo-benzene (1 mmol) and tetrabutylammonium chloride (2 mmol) were dissolved in dimethylacetamide (7 mL) and stirred until all reagents dissolved. Palladium(II) acetate (0.25 mmol) was added and the reaction mixture was stirred at 100 C. for 24 h. The reaction mixture was then cooled to room temperature, diluted with dichloromethane and quenched with water. The organic phase was dried, filtered and concentrated in vacuo, then chromatographed in ethyl acetate in hexanes to yield the desired product.; The following compounds were made in this manner: Example Structure Name Yield 14.1 2-{4-[(2E)-3-(3-cyanophenyl)prop-2- enoyl]piperazine-1-yl}nicotinonitrile 53%

Statistics shows that 3-Iodobenzonitrile is playing an increasingly important role. we look forward to future research findings about 69113-59-3.

Reference:
Patent; AstraZeneca AB; NPS PHARMACEUTICALS; US2007/49578; (2007); A1;,
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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, A new synthetic method of this compound is introduced below., Recommanded Product: 460-37-7

A solution of 2.0 g (5.95 mmol) of the compound from Ex. 21 A in 40 ml DMF was added 1.39 g (13.1 mmol) of cesium carbonate and stirred for 15 min at RT.Then 2.66 g (11.9 mmol) 3,3,3-trifluoro-1-iodopropane were added, and the mixture was heated to 60 C.After 1 hour, additional 2.66 g (11.9 mmol) 3,3,3-trifluoro-1-iodopropane added.Stirring at 60 C was continued for 16 hours.After cooling to RT was treated with about 160 ml of water supply and is extracted three times with 80 ml of diethyl ether.The combined organic extracts were washed with saturated sodium chloride solution.After drying over anhydrous magnesium sulfate, was filtered and evaporated.The crude product was purified by MPLC on a Puriflash cartridge (100 g silica gel, cyclohexane / ethyl acetate 7: 1-> 1: 1).The product fractions were combined, evaporated and the residue dried under high vacuum.There were 1.86 g (72% d. Th.) Of the title compound.

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; BAYER PHARMA AKTIENGESELLSCHAFT; HAERTER, MICHAEL; DELBECK, MARTINA; KALTHOF, BERND; LUSTIG, KLEMENS; LINDNER, NIELS; KAST, RAIMUND; WASNAIRE, PIERRE; SUESSMEIER, FRANK; (372 pag.)TW2016/7950; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, 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 31827-94-8, Computed Properties of C8H6BrIO

General procedure: The appropriate carbonyl compound (50 mmol) was dissolved in 50 mL of ethanol and magnetically stirred with an equimolar quantity of thiosemicarbazide for 24 h at room temperature with catalytic amounts of acetic acid. The desired thiosemicarbazone precipitated from reaction mixture, was filtered, crystallized from suitable solvent, and dried. Equimolar quantities of 4-iodo-acetophenone and bromine, both dissolved in chloroform, were stirred for 4 h at room temperature until the presence of HBr disappeared. The solution was evaporated under vacuum and the obtained pale yellow solid was washed with petroleum ether to give alpha-bromo-4-iodo-acetophenone in good yield (94%). Equimolar amounts of the prepared thiosemicarbazone (50 mmol) and alpha-bromo-4-iodo-acetophenone (50 mmol), both suspended in 50 mL of ethanol, were reacted at room temperature under magnetic stirring for 10 h. The precipitate was filtered and purified by chromatography to give compounds 1-25 in high yield.

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; Secci, Daniela; Bizzarri, Bruna; Bolasco, Adriana; Carradori, Simone; D’Ascenzio, Melissa; Rivanera, Daniela; Mari, Emanuela; Polletta, Lucia; Zicari, Alessandra; European Journal of Medicinal Chemistry; vol. 53; (2012); p. 246 – 253;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

61272-76-2, name is 4-Fluoro-2-iodoaniline, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. COA of Formula: C6H5FIN

7V-Benzyl-5-bromo-2-iodobenzamide (125 mg, 0.30 mmol), 4-fluoro-2-iodoaniline (29 pL, 0.25 mmol), copper(I) iodide (10 mg, 0.05 mmol), and potassium carbonate (86 mg, 0.63 mmol) were taken up in anhydrous DMSO (1.5 mL). The resulting reaction mixture was first stirred at 80 C for 2 hr, followed by heating to 135 C for another 10 hr. After cooling to room temperature, the mixture was diluted with an excess of Et20 and washed with water. The organic layer was dried over NaiSGy filtered and concentrated. The residue was purified by flash column chromatography (EtOAc : Hex = 0 : 100 to 100 : 0; EtOAc : DCM = 0 : 100 to 30 : 70) to give 10-benzyl-2-bromo-8-fluoro-5,10-dihydro-l li7-dibenzo[Z>,e][l,4]diazepin-l l-one (43 mg, 44 %) as a light yellow solid. (0794) NMR (500 MHz, DMSO-de) d 8.06 (s, 1H), 7.74 (d, J = 2.4 Hz, 1H), 7.54 (dd, J = (0795) 2.4, 8.5 Hz, 1H), 7.30 – 7.24 (m, 5H), 7.22 – 7.17 (m, 1H), 7.09 (dd, J= 6.0, 8.7 Hz, 1H), 7.04 (d, ./ 8.9 Hz, 1 H), 6.91 (td, J= 2.7, 8.4 Hz, 1H), 5 26 (s, 2H); LC/MS (ESI) m/z 396.73 [M+H]+.

The synthetic route of 61272-76-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DANA-FARBER CANCER INSTITUTE, INC.; GRAY, Nathanael S.; DE CLERCQ, Dries; JANG, Jaebong; JANNE, Pasi; TO, Ciric; ECK, Michael; PARK, Eunyoung; HEPPNER, David; (0 pag.)WO2019/164949; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 76801-93-9, The chemical industry reduces the impact on the environment during synthesis 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, I believe this compound will play a more active role in future production and life.

(c) (-)-5-Acetamido-2,4,6-triiodo-N,N’-bis(2,3-dihydroxypropyl)-isophthalamide The (-)-compound was prepared from (-)-5-amino-2,4,6-triiodo-N,N’-bis(2,3-dihydroxypropyl)-isophthalamide (14 g) in a similar manner to that described in C(a) above. The product was purified by recrystallisation from water. Yield: 9 g (61%) [alpha]546 =-4.2; [alpha]578 =-3.8 (c=4.5; DMF:H2 O=2:8). Melting point: 287-289 dec. Analysis–Found: C, 25.77; H, 2.72; I, 50.7; N, 5.62. Calc. for C16 H20 I3 N3 O7: C, 25.72; H, 2.70; I, 50.95; N, 5.62.

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, 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nyegaard & Co. A/S; US4250113; (1981); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com