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. 5471-81-8, name is Methyl 4-iodo-3-methylbenzoate, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C9H9IO2

Under a protective atmosphere of inert gas, Pd(OAc)2 (2.2 mg, 10 mol%), XPhos (19.1 mg, 20 mol%), NBE-CO2K (3.5 mg, were added to a 4.0 mL reaction flask equipped with a magnetic stir bar. 10 mol%), methyl 3-methyl-4-iodobenzoate (0.2 mmol, 1.0 equiv.), (8R, 9S, 13S, 14S)-6,7,8,9,11,12,13,14, 15,16-decahydro-13-methyl-3-(((R)-oxiran-2-yl)methoxy)-17H-cyclopenta[a]phenanthrene-17-one(0.6mmol,3.0 equiv.) and dry N-methylpyrrolidone (1.0 mL). The reaction flask was capped and stirred at room temperature for about 5 minutes.The mixture was then heated to 80 C and stirred for 24 hours. After the reaction vessel was cooled to room temperature, it was quenched with water (10 mL).Extract with butyl ether (3 x 10 mL), dry over Na2SO4, Purified by column chromatography, the eluent was dichloromethane.Yield 7-methyl-2-(((8R,9S,13S,14S)-7,8,9,11,12,13,14,15,16,17-decahydro-13-methyl-17 -oxygenGeneration-6H-cyclopenta[a]phenanthr-3-yl)oxy)methyl)-2,3-dihydrobenzofuran-5-carboxylic acid methyl ester 74mg (colorless oilLiquid, yield 78%).

According to the analysis of related databases, 5471-81-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Wuhan University; Zhou Qianghui; Wu Chenggui; Cheng Honggang; (20 pag.)CN108329285; (2018); A;,
Iodide – Wikipedia,
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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 31599-61-8 as follows. SDS of cas: 31599-61-8

General procedure: A 10 mL Schlenk tube was charged with 2-phenylindole 1a (193.2 mg, 1.0 mmol), CuI (10 mol%, 19.0 mg, 0.1 mmol) and K3PO4 (424 mg, 2.0 mmol). The Schlenk tube was evacuated and filled with N2 (this procedure was repeated three times), and then toluene (2.0 mL), DMEDA (20 mol%, 17.6 mg, 0.2 mmol) and iodobenzene 2a (244.8 mg, 1.2 mmol) were added. The resulting mixture was stirred at 110 C for 24 h. After cooling to room temperature, the reaction mixture was quenched and extracted with ethyl acetate (10 mL × 3). The organic extracts were combined, dried over Na2SO4 and concentrated under reduced pressure, and then purified by silica gel chromatograph (petroleum ether) to yield the desired product as a white solid (245.1 mg, 91% yield). The data of compounds 3a-q can be found in Supporting information.

According to the analysis of related databases, 31599-61-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Wei; Han, Li-Ya; Liu, Rui-Li; Xu, Li-Ge; Bi, Yan-Lan; Chinese Chemical Letters; vol. 25; 9; (2014); p. 1240 – 1243;,
Iodide – Wikipedia,
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These common heterocyclic compound, 58313-23-8, name is Ethyl-3-iodobenzoate, 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. Product Details of 58313-23-8

3-Allyl-benzoic acid ethyl ester (18-7).; A -45 C solution of ethyl 3-iodobenzoate (2.434 g, 8.8 mmol) in 40 mL THF was treated with J-PrMgCl (4.8 mL, 9.6 mmol, 2 M/ether). After 1 h, allyl bromide (1.6 mL, 18.9 mmol) was added followed by CuCN (79 mg, 0.88 mmol). The reaction was stirred for 1 h and then was quenched by addition of 50 mL saturated NH4Cl solution. Water (30 mL).was added and the resulting mixture was extracted with ethyl acetate (3 x 50 mL). The combined ethyl acetate solution was dried (MgSO4), filtered and evaporated. Purification by flash chromatography on silica gel (5% ethyl acetate/hexanes -> 10%) gave the title compound (1.145 g, 68%).

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

Reference:
Patent; ALLERGAN, INC.; WO2006/63179; (2006); A1;,
Iodide – Wikipedia,
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Electric Literature of 25245-27-6, 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. 25245-27-6, name is 1-Iodo-3,5-dimethoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a dioxane (2 mL) solution of N-tosylhydrazone (0.24 mmol), tBuOLi (0.53 mmol), Pd2dba3 (0.02 mmol), and XPhos (0.04 mmol) was added the required aryl iodide (0.24 mmol). The mixture was stirred at 90 C for 5 h CH2Cl2 (5 mL) was then added to the cooled mixture which was filtered over a pad of Celite. After concentration, the residue was purified by silica gel chromatography to yield 1a-c, 1k.

The synthetic route of 1-Iodo-3,5-dimethoxybenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Rasolofonjatovo, Evelia; Provot, Olivier; Hamze, Abdallah; Rodrigo, Jordi; Bignon, Jerome; Wdzieczak-Bakala, Joanna; Desravines, Deborah; Dubois, Joelle; Brion, Jean-Daniel; Alami, Mouad; European Journal of Medicinal Chemistry; vol. 52; (2012); p. 22 – 32;,
Iodide – Wikipedia,
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Related Products of 31827-94-8, These common heterocyclic compound, 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, 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: In a typical experimental procedure, o-phenlylenediamine and alpha-bromo ketone in 1:1 molar ratios was taken in a 100 mL round bottom flask. To this water-methanol (1:1) and 100 mg PHP was admixed. The reaction mixture was then allowed to stir with magnetic spinning bar, after some time a yellowish mass appeared which settles down like a precipitate after the completion of the reaction (checked by TLC). It was then filtered; the solid reaction mixture was dissolved with dichloromethane (25 mL) and evaporated under vacuum. The crude product was then crystallised from ethanol. The desired product was pure on TLC and characterized by spectral (IR, 1H and 13C NMR) data and compared to those reported in literature.

The synthetic route of 31827-94-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ghosh, Pranab; Mandal, Amitava; Tetrahedron Letters; vol. 53; 48; (2012); p. 6483 – 6488,6;; ; Article; Ghosh, Pranab; Mandal, Amitava; Tetrahedron Letters; vol. 53; 48; (2012); p. 6483 – 6488;,
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. 29289-13-2, name is 2-Iodo-4-methylaniline, A new synthetic method of this compound is introduced below., Product Details of 29289-13-2

General procedure: A 25 mL reaction tube was charged with 2-haloaniline 1 (0.6 mmol), potassium o-ethyldithiocarbonate 2 (1.8 mmol), FeF3 (0.06 mmol), 2,2?-bis(diphenylphosphino)-1,1?-binaphthyl (0.03 mmol) and DMF (4 mL). The reaction vessel was flushed with argon for three times and sealed. Then the mixture was stirred electromagnetically in an oil bath at 110 for 3 – 21 hours. The reaction process was monitored by TLC on silica gel. After the reaction was completed, the reaction mixture was cooled to room temperature, then 4 mL HCl (3mol/L) was added and stirred for 30 minutes. Then the reaction mixture solution was extracted by ethyl acetate (3*20 mL). Subsequently, the combined organic solution were dried by anhydrous sodium sulfate and the target product was purified by silica gel colum chromatography (eluent: petroleum ether / ethylacetate) to give the corresponding pure product 3.

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; Gao, Min; Lou, Chunqing; Zhu, Ning; Qin, Weijing; Suo, Quanling; Han, Limin; Hong, Hailong; Synthetic Communications; vol. 45; 20; (2015); p. 2378 – 2385;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 263351-43-5, A common heterocyclic compound, 263351-43-5, name is tert-Butyl 3-iodobenzylcarbamate, molecular formula is C12H16INO2, 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: To a solution of N-t-butyloxycarbonyl-4-iodobenzylamine (440 mg,1.30 mmol) in THF was added CuI (125 mg, 0.70 mmol), Et3N (0.40 ml, 2.60 mmol)and Pd(PPh3)4 (53.0 mg, 0.046 mmol) at room temperature. After the stirred for 5 min, 6a (216 mg, 1.30 mmol) was added to the solution. After the stirring for 24 h, saturatedNH4Cl and Et2O were added to the solution. Organic layer was washed with saturatedNaHCO3 and brine, dried over MgSO4 and evaporated in vacuo. The residue waspurified by column chromatography (hexane:AcOEt=1:1) to give 11 (121 mg, 0.30mmol, 25%) as a colorless oil.

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; Konno, Hiroyuki; Sato, Taki; Saito, Yugo; Sakamoto, Iori; Akaji, Kenichi; Bioorganic and Medicinal Chemistry Letters; vol. 25; 22; (2015); p. 5127 – 5132;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 82998-57-0, 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. 82998-57-0, name is 3-Iodo-4-methylbenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

3-Iodo-4-methyl-N-(3-(4-methyl-1H-imidazol-1-yl)-5-(trifluoromethyl)phenyl)Benzamide: 3-Iodo-4-methylbenzoic acid (2.62 g, 10 mmol) was refluxed in soc2 (10 mL) for 5 1 h. The volatile components were removed on a rotavap and the residue was dissolved inbenzene (10 mL), concentrated to dryness on a rotavap and further dried under vacuum. The resulting acyl chloride was added to a solution 3-(4-methyl-IH-imidazol-I-yl)-5- (trifluoromethyl)benzenearnine (2.46 g, 10.2 mmol), N,N-diisopropylethylamine (1.56 g, 12 mmol), and a catalytic amount of DMAP in THF (20 mL). After stirring at rt for 2 h, the reaction10 was quenched with water. EtOAc was added and the layers separated. The combined organic layers were concentrated to dryness and used without purification in next step.

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-Iodo-4-methylbenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ARIAD PHARMACEUTICALS, INC.; GOZGIT, Joseph, M.; RIVERA, Victor, M.; SHAKESPEARE, William, C.; ZHU, Xiaotian; DALGARNO, David, C.; WO2013/162727; (2013); 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 624-76-0 as follows. COA of Formula: C2H5IO

Example 396 (Z)-3-(2-Hydroxyethyl)-5-[{7-(4-methoxyphenyl)furo[3,2-c]pyridin-2-yl}methylene]thiazolidine-2,4-dione Step 1: Synthesis of 3-(2-hydroxyethyl)thiazolidine-2,4-dione Thiazolidinedione (12.8 mmol), 2-iodoethanol (15.1 mmol), potassium carbonate (17.4 mmol) and tetrabutylammonium iodide (1.3 mmol) were placed in acetone (25 ml), and stirred at 40 C. for 10 hours. The reaction mixture was cooled to room temperature, filtered through Celite, and concentrated under reduced pressure to yield brown oil. The residue thus obtained was purified by silica gel column chromatography (n-hexane/ethyl acetate=4/1, v/v) to obtain the title compound as colorless oil (yield: 54%). 1H NMR (CDCl3, 400 MHz) delta 4.00 (s, 2H), 3.85 (brs, 4H), 1.94 (brs, 1H)

According to the analysis of related databases, 624-76-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; YUHAN CORPORATION; Seo, Hyoung Sig; Kim, Tae Kyun; Lee, Hyun Joo; Kim, Dong Hoon; Lee, Gyu Jin; Park, Jun Chul; Gal, Ji Yeong; Kim, Tae-hoon; Hyun, Kwan Hoon; Ahn, Kyoung Kyu; Park, Kaapjoo; Nam, Su Youn; Lee, Ge Hyeong; Lim, Hee Jong; US2015/191478; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 56096-89-0, name is 4-Fluoro-2-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. Recommanded Product: 4-Fluoro-2-iodobenzoic acid

General procedure: To a stirred solution of 2-iodobenzoic acids a (10 mmol) in CH2Cl2, was added DCC (dicyclohexylcarbodiimide, 11 mmol), DMAP (Dimethylaminopyridine, 2 mmol) and alcohols b (10 mmol) in sequence. The resulting solution was stirred overnight at room temperature then filtered through a sand core funnel and washed with diethyl ether (2 x 40mL). The combined organic layers were washed with water, brine, dried over Na2SO4, and concentrated under reduced pressure. The crude material was purified by flash column chromatography to obtain the pure product c in moderate to good yields. To a soluton of 2-iodobenzoates c in Et3N (5 mL) was added PdCl2 (PPh3)2 (4 mol %) and CuI (2 mol %) and the reaction vial was flushed with Ar and the reaction mixture was stirred for 5 minutes. A solution of propargyl alcohols d (1.05 equiv) in Et3N (5 mL) were then added dropwise through a syringe for 5 minutes. The resulting solution was stirred at room temperature overnight. When the reaction was considered complete as determined by TLC analysis, the mixture was quenched by addition of saturated aqueous ammonium chloride (10 mL) and extracted with ethyl ether (3 x 40 mL). The combined organic layers were washed with water, brine, dried over Na2SO4, and concentrated under reduced pressure. The crude material was purified by flash column chromatography to give 1.

The synthetic route of 4-Fluoro-2-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhu, Hai-Tao; Tong, Xiao-Juan; Zhou, Ni-Ni; Yang, De-Suo; Fan, Ming-Jin; Tetrahedron Letters; vol. 57; 49; (2016); p. 5497 – 5500;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com