Month: June 2021

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. 6940-76-7, name is 1-Chloro-3-iodopropane, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 6940-76-7

General procedure: In a round flask 300 mg (1.18 mmol) of compound 1 are weighed and placed in an inert atmosphere with a magnetic stirrer. Then, 3 ml of dry THF are added and the system is cooled to 0 C. Then 1.2 equivalents of LDA are added and left in an ice bath for 10 minutes. The ice bath is removed and left under constant stirring for 2 hours. The round flask is cooled again to 0 C and 1,3-chloroiodopropane is added using a syringe previously purged with nitrogen. The ice bath is removed and the reaction is followed by TLC until the consumption of the starting material (1). Once the reaction (approximately 2.5 h) is finished, 0.5 ml of a saturated NH4OH solution is added and an extraction with 5 ml of dichloromethane is carried out in triplicate, the organic phase is collected and dried with anhydrous sodium sulfate, once dried the organic phase is distilled under vacuum. The purification is carried out by a chromatographic column using silica gel as a stationary phase and a mixture of Hexane and ethyl acetate in a proportion of 95:5. A pale yellow oil is obtained in all cases.

According to the analysis of related databases, 6940-76-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Xavier Dominguez-Villa, Francisco; Avila-Zarraga, Gustavo; Armenta-Salinas, Concepcion; Tetrahedron Letters; vol. 61; 15; (2020);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 19094-56-5, These common heterocyclic compound, 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, 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.

To a dried flask, 5-iodo-2-chlorobenzoic acid (20.0 g, 70.8 mmol) and dichloromethane (60 mL) were added. The reaction mixture was stirred, then oxalyl chloride (9.8 g, 77.9 mmol) and DMF (0.2 mL) were slowly added dropwise, and some bubbles were observed. The reaction mixture was stirred at room temperature for 7 hours. The solvent and excess oxalyl chloride were removed by rotary evaporation to give a gray solid, which was used directly in the next step without further purification.

The synthetic route of 19094-56-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangsu Hansoh Pharmaceutical Co., Ltd.; ZHONG, Huijuan; LIAO, Jianchun; YU, Hongping; XU, Yaochang; LI, Qing; CHEN, Jianghua; GAO, Peng; TAN, Songliang; WANG, Shaobao; (45 pag.)US2016/222047; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 56096-89-0,Some common heterocyclic compound, 56096-89-0, name is 4-Fluoro-2-iodobenzoic acid, molecular formula is C7H4FIO2, 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 5a (5.0 g, 18.8 mmol, 1.0 eq), 5b (4.60 g, 28.2 mmol, 1.5 eq), potassium carbonate (6.5 g, 47.0 mmol, 2.5 eq), copper powder (360.0 mg, 5.64 mmol, 0.3 eq), and Copper(I) oxide (810.0 mg, 5.64 mmol, 0.3 eq) in DMF (100.0 mL) was stirred at 140 C overnight under argon atmosphere, then cooled to room temperature. Water (50.0 mL) was added. The mixture was filtered through ceiite. The filtrate was acidified to pH===2 with 2 N HC1, then water (50.0 mL) was added. The resulting mixture was extracted with EtOAc (50 0 ml, x 3). The combined organic layers were washed with brine (20.0 mL x 5), dried over anhydrous NaiSOr and filtered. The filtrate was concentrated in vacuo to afford crude 5c (3.0 g, 54.0 %). LC/MS: 300.0 [M+H]+.

The synthetic route of 56096-89-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SILICON SWAT, INC.; CHAMBERLAIN, Brian T.; RICE, James M.; JERNIGAN, Finith E., III; SHERMAN, Woody; KULKARNI, Meghana M.; SHECHTER, Sharon; ALLEN, Bryce K.; TAN, Dazhi; MARINO, Kristen A.; LIN, Zhixiong; (292 pag.)WO2019/100061; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, 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. Safety of 1-Iodo-2-(trifluoromethyl)benzene

C. To a degassed sample of 4-methylenepiperidine-1-carboxylic acid tert- butyl ester (0.527 g, 2.67 mmol) was added 9-borabicyclic[3,3,1]nonane (5.6 mL of a 0.5 M solution in THF, 2.8 mmol). The resulting solution was refluxed for 1 hour. After cooling to ambient temperature, the solution was added to a mixture of 1-iodo-2- trifluoromethylbenzene (0.707 mg, 2.600 mmol), Pd-catalyst (3 molpercent), DMF (25 mL), water (1 mL), and K2CO3 (0.6 g). The resulting mixture was heated at 600C for 3 hours. The mixture was cooled to ambient temperature and then poured into water. The pH of the solution was adjusted to 11 with 10percent NaOH solution and the mixture was extracted with ethyl acetate. The combined organic extracts were washed with brine and dried over Na2SO4, filtered, and evaporated to give a crude oil, which was further purified by column chromatography to afford 4-(2- trifluoromethylbenzyl)piperidine-1-carboxylic acid te/t-butyl ester as a waxy solid (0.638 g) in 70 percent yield.

The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; XENON PHARMACEUTICALS INC.; WO2006/34338; (2006); 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. 63262-06-6, name is 1,4-Dibromo-2,5-diiodobenzene, A new synthetic method of this compound is introduced below., Recommanded Product: 63262-06-6

Under a nitrogen atmosphere, to a 50mL three-necked flask 1,4-dibromo-2,5-di-iodobenzene 219 mg (0.45 mmol) and diethyl ether (5 ml) was added and cooled to -78 C..Thereafter, it was added dropwise n- butyllithium 0.54ml at the same temperature (1.66 M hexane solution, 0.90 mmol), and stirred for 1 hour.At Thereafter the same temperature, it was added dropwise synthesized bis previous step was dissolved in diethyl ether (1ml) (2-n- hexyl-4-thienyl) disulfide 359 mg (0.90 mmol), and stirred at room temperature for 12 hours.The reaction by the addition of water was stopped, after extraction with diethyl ether, and the organic layer was dried over anhydrous sodium sulfate.And concentrated under reduced pressure, the resulting residue was purified by silica gel column chromatography (hexane), 1,4-bis [(2-n-hexyl-4-thienyl) sulfanyl] of 2,5-dibromobenzene yellow solid 228mg was obtained (80% yield).

The synthetic route of 63262-06-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TOSOH CORPORATION; HACHIYA, HITOSHI; WATANABE, MAKOTO; UEDA, SAORI; (16 pag.)JP2015/227297; (2015); A;,
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. 123158-75-8, name is 4-Chloro-2-iodo-6-nitroaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 123158-75-8

Preparation 41: 5-Chloro-3-phenyl-7-nitro-1H-indoleStep A: 5-Chloro-7-nitro-3-phenyl-2-trimethylsilyl-1H-indole; 2-Amino-5-chloro-3-nitro-phenyliodide (1.5 g, 4.90 mmol) prepared in Preparation 19 and 1-phenyl-2-trimethylsilylacetylene (4.3 g, 24.50 mmol) were dissolved in DMF (50 mL). Palladium acetate (0.11 g, 0.5 mmol), lithium chloride (0.21 g, 4.90 mmol) and triethylamine (2.48 g, 24.50 mmol) were added thereto, and the mixture was stirred under heating for 3 h to 100 C. After completion of the reaction, water was added to the reaction mixture, which was then extracted with ethyl acetate, washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and filtered. The solvent was removed under reduced pressure, and the residue was purified by column chromatography to give the title compound (1.05 g, Yield 87%).1H-NMR (400 MHz, CDCl3); delta 9.78(br s, 1H), 8.15(s, 1H), 7.78(s, 1H), 7.387.48(m, 5H), 0.26(s, 9H)

The synthetic route of 123158-75-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LG Life Sciences Ltd; US2010/197673; (2010); 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. 105202-02-6, name is 2-Iodo-5-(trifluoromethyl)aniline, A new synthetic method of this compound is introduced below., SDS of cas: 105202-02-6

General procedure: 2-aminobenzenethiol (10 g, 80mmol), 3, 4-difluorobenzonitrile (11.12, 80mmol) and ferric citrate (19.59g, 80mmol) were added in DMF (50.00 mL) at 25-30 0C. The reaction mixture was heated to 110C. Reaction mixture was monitored for the synthesis of compound 3 by TLC. (2ml of reaction mixture was withdrawn and separated in ethylacetate and water. Ethyl acetate solution concentrated and crystallised in isopropyl ether to give compound 3 for characterization). After completion of reaction by TLC, powdered potassium carbonate (16.58 g, 120mmol) was added to the solution and stirred for 1 hr. The mixture was heated to 110C till completion by TLC. After completion of reaction, the mass was cooled to 25-30 C. Ethyl acetate (150 mL) and DM water (150 mL) were added. Layers separated. Organic layer washed with water (150 mL), dried over sodium sulfate and concentrated. Isopropyl ether (IPE; 150 mL) was added to the slurry, filtered, washed with IPE. Dried under vacuum at 50 C (16.84g, 94%).

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; Das, Tonmoy Chitta; Quadri, Syed Aziz Imam; Farooqui, Mazahar; Letters in Organic Chemistry; vol. 16; 1; (2019); p. 16 – 24;,
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 4897-68-1 as follows. SDS of cas: 4897-68-1

Step 40a. 2-(2-Bromo-5-methoxyphenylthio)-1-(4-methoxybenzyl)-1H-imidazo[4,5-c]pyridin-4-amine (Compound 0205-53) A mixture of compound 0204 (1.549 g, 5.41 mol), 1-bromo-2-iodo-4-methoxybenzene (Compound 0104-13) (2.54 g, 8.115 mol), neocuproine hydrate (113 mg, 0.541 mmol), CuI (103 mg, 0.541 mmol) and NaOt-Bu (519 mg, 5.41 mmol) in anhydrous DMF (50 mL) was stirred for 24 h at 110 C. (oil bath) under nitrogen atmosphere. The solvent was removed under high vacuum and the crude purified by column chromatography on silica gel (CH2Cl2/MeOH at 100/1) to give the title compound 0205-53 as a brown solid (1.67 g, 65%): LCMS: 471 [M+1]+.

According to the analysis of related databases, 4897-68-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Cai, Xiong; Qian, Changgeng; Zhai, Haixiao; US2008/234314; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 3032-81-3,Some common heterocyclic compound, 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, molecular formula is C6H3Cl2I, 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.

To a 3-neck 1 L reactor equipped with temperature probe, overhead stirrer, reflux condenser, and nitrogen bubbler, was added copper (I) iodide (4.0 g, 0.021 mol), 2-picolinic acid (5.2 g, 0.042 mol), 3,5-dichloroiodobenzene (99 g, 0.36 mol), and cesium carbonate (233 g, 0.72 mol) under nitrogen. Dioxane (600 mL) and dimethyl malonate (91 g, 0.69 mol, 1.9 eq.) were then added to the solid mixture with stirring under nitrogen. The resulting mixture was then heated to 90 C for 7 h, forming a pale yellow-green slurry. Water (300 mL) and hexanes (200 mL) were added to the cooled reaction mixture at room temperature, stirred for 5 min, and transferred to a separatory funnel, and extracted twice with 75 mL dioxane-hexanes (2: 1). The combined organic phases were washed with saturated aqueous ammonium chloride (200 mL) and concentrated to dryness to remove all dioxane. The residue was mixed with MeOH ( 100 mL) and water (200 mL). After stirring for 30 min, the mixture was cooled to 0 C with an external ice-water bath and slowly stirred for 2 h. Filtration gave 98.6 g of crude material which was dissolved in MeOH ( 160 mL) at 50 C, with stirring, cooled to 0 C over 6 h then maintained at 0 C for 2 h. Filtration gave 85.6 g of the title compound as a fine white crystalline solid. The filtrate was concentrated to remove all MeOH, and the residue was filtered to give an additional 4.12 g of the title compound for a combined 89% yield.

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-Dichloro-5-iodobenzene, its application will become more common.

Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; ZHANG, Wenming; ANNIS, Gary David; WO2013/90547; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 627-31-6, A common heterocyclic compound, 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), molecular formula is C3H6I2, 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.

Sodium hydride 60% in oil (0.43 g, 10.7 mmol) was added to a suspension of Iota,Gamma trimethylenebisthymine (1.51 g, 5.1 mmol) in dimethyl sulfoxide (80 mL) and stirred overnight at 60-65 C. 1, 3-Diiodopropane (1.63 g, 4.8 mmol) was added to the reaction mixture and stirred for 3 days at 80 C to give a clear solution. The solvent was evaporated; the residual solid was washed with potassium carbonate aqueous solution (30 mL), methanol (20 mL), and diethyl ether (20 mL). The product in was purified by silica gel column using ethyl acetate/ methanol as eluents to give the cyclic compound, II as a white solid (0.204 g, 12% ). H NMR (600 MHz, CDC13, ppm) : 7.05 (s, 2H, C6-H), 4.07 (t, 3H, N3-CH2), 3.75 (t, 4H, N1-CH2), 2.15(t, 2H, N3- C-CH2), 1.98 (t, 2H, N1-C-CH2), 1.89 (s, 6H, C5-CH3); 13C NMR (150 MHz, CDC13): 164.11, 152.53, 141.21, 108.15, 51.20, 45.73, 28.20, 26.35, 10.35; Mass (APCI-Neg): 331.13 (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; REGENTS OF THE UNIVERSITY OF MINNESOTA; VINCE, Robert; RAZA, Abbas; DREIS, Christine; WO2013/106728; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com