Category: iodides-buliding-blocks

Reference of 774608-49-0,Some common heterocyclic compound, 774608-49-0, name is 4-Bromo-1-chloro-2-iodobenzene, molecular formula is C6H3BrClI, 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 flame dried round bottom flask was charged with 4-bromo-l-chloro-2- iodobenzene (33.1 g, 104 mmol) and Et20 (206 mL). The solution was cooled to -78 C and a solution of n-butyllithium solution (2.5 M in hexanes, 41.7 mL, 104 mmol) was added dropwise. The reaction mixture was stirred at -78 C for 15 minutes. A second, flame dried round bottom flask was charged with a solution of 4-(fluoromethyl)-2-oxa-3- azabicyclo[3.1.0]hex-3-ene (6c rac; 6 g, 52.1 mmol) in toluene (229 mL) and cooled to-78 C. Boron trifluoride diethyl etherate (6.61 mL, 52.1 mmol) was added, the reaction mixture was stirred for 5 minutes at – 78 C and added via cannula to the aryllithium species. The reaction mixture was stirred at -78 C for 10 minutes. The reaction was quenched with saturated ammonium chloride solution and warmed to RT. The reaction mixture was diluted with water and EtOAc. The organic layer was separated and the aqueous layer was washed with additional EtOAc. The combined organic layers were A-1813-WO-PCT – 101 – washed with brine and dried over magnesium sulfate. The filtrate was concentrated under reduced pressure and the crude material was purified via silica gel chromatography, eluting with 5-45% EtOAc:Hexanes to afford the title compound (10.19 g, 33.2 mmol, 63.8 % yield). MS m/z = 305.9 [M+H]+. Calculated for CnH10BrClFNO: 306.6

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Bromo-1-chloro-2-iodobenzene, its application will become more common.

Reference:
Patent; AMGEN INC.; MINATTI, Ana Elena; LOW, Jonathan, D.; ALLEN, Jennifer, R.; AMEGADZIE, Albert; BROWN, James; FROHN, Michael, J.; GUZMAN-PEREZ, Angel; HARRINGTON, Paul, E.; LOPEZ, Patricia; MA, Vu Van; NISHIMURA, Nobuko; QIAN, Wenyuan; RUMFELT, Shannon; RZASA, Robert, M.; SHAM, Kelvin; SMITH, Adrian, L.; WHITE, Ryan; XUE, Qiufen; WO2014/138484; (2014); A1;,
Iodide – Wikipedia,
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Related Products of 696-41-3,Some common heterocyclic compound, 696-41-3, name is 3-Iodobenzaldehyde, molecular formula is C7H5IO, 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.

Reference Example 136 tert-butyl ({4-(2-fluorophenyl)-5-[(3-formylphenyl)thio]-1,3-thiazol-2-yl}methyl)methylcarbamate To a solution of 2-ethylhexyl 3-{[2-{[(tert-butoxycarbonyl)(methyl)amino]methyl}-4-(2-fluorophenyl)-1,3-thiazol-5-yl]thio}propanoate (749 mg) in ethanol (10 mL) was added sodium ethoxide (381 mg) at 0 C., and the mixture was stirred at room temperature for 4 hr, and concentrated under reduced pressure. A mixture of the residue, 3-iodobenzaldehyde (489 mg), tris(dibenzylideneacetone)dipalladium(0) (35 mg) and 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthine (81 mg) in toluene (10 mL) was stirred at 80 C. for 3 hr. The reaction mixture was allowed to cool to room temperature, water was added, and the mixture was extracted with ethyl acetate. The extract was washed successively with saturated aqueous sodium hydrogen carbonate solution, water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=4:1) to give the title compound as a yellow oil (676 mg, yield quantitative). 1H-NMR (CDCl3) delta: 1.47 (9H, brs), 3.00 (3H, brs), 4.69 (2H, brs), 7.10-7.20 (3H, m), 7.34-7.50 (3H, m), 7.65-7.68 (2H, m), 9.90 (1H, s).

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

Reference:
Patent; Takeda Pharmaceutical Company Limited; US2009/156642; (2009); A1;,
Iodide – Wikipedia,
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Related Products of 1437316-91-0, A common heterocyclic compound, 1437316-91-0, name is 2,4-Difluoro-3-iodoaniline, molecular formula is C6H4F2IN, 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 solution of 2,4-difluoro-3-iodoaniline (255 mg, 1 mmol) in 1,2_dichloroethane (3 mL) was slowly added dropwise a solution of P to pyridine (lmL), propylsulfonyl chloride (157 mg, 1. lmmol). The reaction solution was heated under reflux for 2 hours, cooled and concentrated in vacuo to remove the solvent. The resulting oil was dissolved in ethyl acetate (20 mL) and washed with 5% sodium bicarbonate solution, water and saturated brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give N- (2,4-difluoro-3- Iodophenyl) propane-1-sulfonamide (298 mg, 83%).

The synthetic route of 1437316-91-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Beijing Sai Lintai Pharmaceutical Co., Ltd.; Zhengda Tianqing Pharmaceutical Group Co., Ltd.; Xiao Dengming; Li Jijun; Zhu Yan; Hu Yuandong; Wang Huting; Wang Zhe; Wang Zanping; Wei Yongheng; Sun Yinghui; Wu Qiong; Zhang Hui; Peng Yong; Kong Fansheng; Sun Ying; Luo Hong; Han Yongxin; (64 pag.)CN103102349; (2017); B;,
Iodide – Wikipedia,
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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. 41252-96-4, name is 2-Chloro-1-iodo-4-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows., name: 2-Chloro-1-iodo-4-nitrobenzene

General procedure: 4-acryloyloxy-2,2,6,6-tetramethylpiperidin-1-oxyl (3, 0.113 g,0.5 mmol), aryl iodide (4a-i, 0.5 mmol), Bu4N+AcO- (hygroscopic)(0.3 g), PdEnCatTOTP30 (0.0625 g, 0.025 mol,5 mol %), and toluene (2 mL) were placed in a flask, stirred and heated at 80-100 C for 20-27 h under argon. The particular temperatures and times of the reactions are summarized in Table 1. After approximately 6 h, a second portion of a catalyst(0.0625 g, 0.025 mol, 5 mol %) was added. The progress of the reaction was monitored by TLC (silica, hexane/ethyl acetate9:1). Upon completion of the reaction, the solids were filtered off, the dark filtrate was concentrated under reduced pressureand subjected to column chromatography (hexane/ethyl acetate 9:1, benzene/ethyl acetate 95:5, benzene/methanol 95:5 aspossible mobile phases). The red zone was collected, the eluate was evaporated under reduced pressure to yield red oils (solidifiedin a refrigerator), or directly red crystals of 5a-i.

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 41252-96-4.

Reference:
Article; Zakrzewski, Jerzy; Huras, Bogumila; Beilstein Journal of Organic Chemistry; vol. 11; (2015); p. 1155 – 1162;,
Iodide – Wikipedia,
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2401-21-0, name is 1,2-Dichloro-3-iodobenzene, 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. name: 1,2-Dichloro-3-iodobenzene

G. 17alpha-Chloro-17beta-(3′,4′-Dichlorobenzylsulfinyl)-1,4-Androstadiene-3,11-Dione In a manner similar to that described in Example 2A, react 0.238 gms. of 17alpha-(3′,4′-dichlorobenzylthio)-1,4-androstadiene-3,11-dione, 8 ml. of pyridine, 2 ml. of water and 0.411 gm. of iodobenzene dichloride. Purify the residue utilizing thin layer silica gel chromatography, developing with ethyl acetate/chloroform (1:4) and eluding with ethyl acetate. Crystallize the major band from ether to obtain the title compound; m.p.=249¡ã-251¡ã C.

The synthetic route of 2401-21-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Schering Corporation; US4183924; (1980); A;,
Iodide – Wikipedia,
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Related Products of 7681-82-5, 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. 7681-82-5, name is Sodium iodide belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of propionic acid (10 ml), sodium iodide (3.0 g, 20 mmol) and Fe3+- montmorillonite catalyst (0.5 g) were stirred in a round-bottomed flask at 25 C for 6 h. The reaction mixture was filtered off to separate the catalyst. The resultant filtrate was titrated with 0. 1M sodium thiosulphate solution using starch as an indicator to know the amount of iodine present in the solution. The amount of iodine liberated in the reaction is 0.998 g (3.7 mmol)

The synthetic route of Sodium iodide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH; WO2004/50622; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 31599-61-8,Some common heterocyclic compound, 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, molecular formula is C8H9I, 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: An appropriate phenylacetamide (0.12 mmol, 1 equiv), an appropriate iodo compound (0.48 mmol, 4 equiv), Pd(OAc)2 (2.7 mg, 10 mol%), and AgOAc (50 mg, 0.3 mmol, 2.5 equiv) in anhydrous toluene (3 mL) was heated at 110 C for 24 h under a nitrogen atmosphere. After the reaction period, the solvent was evaporated in vacuo to afford a crude reaction mixture. Purification of the crude reaction mixture by column chromatography furnished the corresponding arylated products 4a-q/7a-f (bis arylation products), 3o,r/6a,b/8e,f/9a,b (mono arylation products) (see corresponding Tables/Schemes for specific examples and reaction conditions).

The synthetic route of 31599-61-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bisht, Narendra; Babu, Srinivasarao Arulananda; Tetrahedron; vol. 72; 39; (2016); p. 5886 – 5897;,
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. 216393-67-8, name is 4-Chloro-2-fluoro-6-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C6H4ClFIN

General procedure: To a 50 mL oven-dried flask containing a magnetic stirring bar, Pd(PPh3)2Cl2 (14.0 mg, 0.02 mmol, 1.0 mol %), CuI (2.0 mg, 0.01 mmol, 0.5 mol %), 4-(tert-butyl)-2-iodoaniline (550.0 mg, 2.0 mmol), 2 (317.0 mg,2.2 mmol) [26], and Et3N (10 mL) were added in sequence under argon atmosphere at room temperature. The resulting reaction mixture was stirred for 5 h, then the reaction mixture was filtered through a shortpad of celite, and the solid was washed with EtOAc (20 mL). The combined organic phase was concentrated under reduced pressure, andthe residue was purified by column chromatography on silica gel(eluent: petroleum ether/ethyl acetate=10:1) to afford pure product4c in 75% yield.

The synthetic route of 216393-67-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chang, Sai-Lan; Qiu, Li-Hua; Sun, Ru; Yang, Ling; Ge, Jian-Feng; Dyes and Pigments; vol. 160; (2019); p. 58 – 63;,
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. 25245-27-6, name is 1-Iodo-3,5-dimethoxybenzene, A new synthetic method of this compound is introduced below., Computed Properties of C8H9IO2

General procedure: A mixture of the styrene (3 mmol), the halogenated benzene (3 mmol), triethanolamine (3 mmol) and Pd (II) acetate (0.03 g) was stirred under argon at 100 C for 24 h. The reaction was cooled to 25 C, quenched by the addition of dil. aq. hydrochloric acid (2 N, 10 ml), and extracted with ether (3 ¡Á 100 ml). The organic phases were dried (Na2SO4), the solvents evaporated, and the crude product was subjected to chromatography (silica gel, hexane/ethyl acetate mixtures).

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; Csuk, Rene; Albert, Sabrina; Siewert, Bianka; Schwarz, Stefan; European Journal of Medicinal Chemistry; vol. 54; (2012); p. 669 – 678;,
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. 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C7H5IO2

[00212] 8.1 mg of Pd(OAc)2 (0.036 mmol) and 16 mg (0.033 mmol) of bis(1,2-diphenylarsino)ethane were placed in a reaction tube under nitrogen together with 4 ml of dioxane and 0.45 ml of triethylamine. The tube was heated in an oil bath at 80 C. for 15.5 h and the yellow solution became brown in colour. Then added at room temperature 262 mg (1.06 mmol) of 1-iodo-3,4-methylenedioxybenzene and 0.22 ml (1.5 mmol) of pinacolborane. The reaction mixture was then warmed to 80 C. After 3 h, 45% of the total peak areas was due to the desired product. This increased to 73% after 24 h.

The synthetic route of 5876-51-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Commonwealth Scientific and Industrial Research Organisation; US6680401; (2004); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com