Tag: M.W=200-300

Electric Literature of 103962-05-6, 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. 103962-05-6 name is 1-Iodo-4-(trifluoromethoxy)benzene, 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.

To a solution of 1-iodo-4-(trifluoromethoxy)benzene (15.0 g, 52.0 mmol) in dimethylformamide (90 mL) and water (10 mL) was added 3-(4-bromophenyl)-1H-1,2,4-triazole (C51) (11.0 g, 49.0 mmol), cesium carbonate (34.0 g, 104 mmol), copper(I) iodide (2.80 g, 14.7 mmol), and 8-hydroxyquinoline (2.20 g, 15.0 mmol), and the solution was heated at 140° C. for 8 hours. The cooled solution was decanted from a layer of solid, diluted with a ammonium hydroxide (1N, 100 mL) solution, and extracted with of diethyl ether (2*100 mL). The combined organic layer was dried and concentrated, and the brown solid was eluted through a short silica gel column using 20percent ethyl acetate/hexanes as eluent to give the title compound as a light tan solid (9.50 g, 50percent): mp 111-113° C., 1H NMR (400 MHz, CDCl3) delta 8.56 (s, 1H), 8.07 (d, J=8.6 Hz, 2H), 7.79 (d, J=8.8 Hz, 2H), 7.62 (d, J=8.6 Hz, 2H), 7.39 (d, J=8.8 Hz, 2H); ESIMS m/z 384 ([M+H]+).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Iodo-4-(trifluoromethoxy)benzene, and friends who are interested can also refer to it.

Reference:
Patent; DOW AGROSCIENCES LLC; Fischer, Lindsey G.; Baum, Erich W.; Crouse, Gary D.; DeAmicis, Carl; Lorsbach, Beth; Petkus, Jeff; Sparks, Thomas C.; Whiteker, Gregory T.; US2014/274688; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 455-13-0, 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. 455-13-0, name is 4-Iodobenzotrifluoride, This compound has unique chemical properties. The synthetic route is as follows.

Multi function cap round bottom 4-trifluoromethyl-iodobenzene to 250 ml (5.00g, 18.38mmol), imidazole (1.75g, 25.73mmol), Copper iodide (0.70g, 3.68mmol), Cesium carbonate (11.98g, 36.76mmol), Dimethylformamide (120 ml) for inserting and removing, adaptation stirring time 24 in the curved reflection 110. After reaction, bleeding of the volatiles of decompressing to a cutting, residue column in hexane and a ethylacetate crow mart yes blood section. The again 3A compound (3.12g, 14.71mmol) a obtained.

The chemical industry reduces the impact on the environment during synthesis 4-Iodobenzotrifluoride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; LG Display Co.,Ltd; Lee, Sung Jae; Yang, Jung Hwan; Choe, Hyung Jong; Bae, Suk Young; Haw, Hay Ryeong; Kim, Chun Gi; (30 pag.)KR2016/14205; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 351003-36-6,Some common heterocyclic compound, 351003-36-6, name is 2-Fluoro-5-iodobenzonitrile, molecular formula is C7H3FIN, 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 solution of tert-butyl 4-ethynyl-4-hydroxypiperidine-1-carboxylate (8.2 g, 36 mmol) and 2-fluoro-5-iodobenzonitrile(8.72 g, 43.6 mmol) in N,N-diethylamine (200 mL), was added tetrakis(triphenylphosphine)palladium dichloride(0.80 mg) and copper (I) iodide (0.34 mg). The mixture was stirred at room temperature under N2 for 12 h and thenevaporated. The residue was partitioned between water and EtOAc. The combined organic solutions were washed withbrine (500 mL), dried (Na2SO4), filtered and concentrated to provide tert-butyl 4-[(3-cyano-4-fluorophenyl)ethynyl]-4-hydroxypiperidine-1-carboxylate which was used directly in the next step without further purification.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Fluoro-5-iodobenzonitrile, its application will become more common.

Reference:
Patent; Merck Sharp & Dohme Corp.; WALSH, Shawn; PASTERNAK, Alexander; CATO, Brian; FINKE, Paul, E.; FRIE, Jessica; FU, Qinghong; KIM, Dooseop; PIO, Barbara; SHAHRIPOUR, Aurash; SHI, Zhi-Cai; TANG, Haifeng; (136 pag.)EP2755656; (2016); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 444-29-1, 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. 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A solution of Ar3In or (RC?C)3In (0.37mmol, ca. 0.18M in dry THF) was added to a mixture of MCM-41-N,N-Pd(0) (25mg, 1molpercent) and aryl iodide (1mmol) in dry THF (2mL) under Ar. The resulting mixture was refluxed under Ar until the starting material had been consumed (TLC). After being cooled to room temperature, the mixture was diluted with Et2O (30mL) and filtered. The palladium catalyst was washed with DMF (2×5mL), Et2O (2×5mL) and reused in the next run. The filtrate was washed with sat. aq NaHCO3 (5mL), water (3×10mL) and dried over MgSO4, filtered, and concentrated under vacuum. The residue was purified by flash chromatography on silica gel to give the desired cross-coupling product.

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; Lei, Zhiwei; Liu, Haiyi; Cai, Mingzhong; Journal of Organometallic Chemistry; vol. 852; (2017); p. 54 – 63;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. Quality Control of 1,3-Dichloro-5-iodobenzene

EXAMPLE 31 1-(3,5-Dichlorophenyl)-3-methyl-1-butyn-3-ol A mixture of 25.5 g (0.094 mole) of 3,5-dichloroiodobenzene, 550 ml dry triethylamine, 12 g (0.14 mole) of 2-methyl-2-hydroxy-3-butyne, 0.42 g (0.0019 mole) palladium (II) acetate, and 1 g (0.0038 mole) of triphenylphosphine was heated to reflux under nitrogen for four hours. The resulting mixture was cooled, diluted with ether and washed with two 500-ml portions of 3N hydrochloric acid. The ether layer was separated, dried over anhydrous magnesium sulfate, and evaporated in vacuo to yield the crude product as an oily residue. The purified product was obtained by distillation to yield 7.95 g, bp 115°-125° C./0.0001 mm.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3032-81-3, its application will become more common.

Reference:
Patent; McNeilab, Inc.; US4898889; (1990); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 3058-39-7, 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. 3058-39-7, name is 4-Iodobenzonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Phenylpropiolic acid (43.8 mg, 0.3 mmol), iodobenzene (61.2 mg, 0.3 mmol), Na2CO3 (47.6 mg, 0.45 mmol), NaCuY (12 mg, 0.03 mmol) were added to a vial under DMSO (1.0 mL). The resulting mixture was heated to 100 °C for 12 h under vigorous stirring. After complete reaction, the reaction mixture was treated with water and extracted with EtOAc. The organic layer was dried under MgSO4 and concentrated by using vacuum evaporation. The crude mixture was purified by column chromatography.

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, 4-Iodobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Park, Jaerim; Jung, Dasom; Kim, Han-Sung; Na, Kyungsu; Lee, Sunwoo; Catalysis Communications; vol. 99; (2017); p. 83 – 88;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 626-62-0, name is Iodocyclohexane, 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. Safety of Iodocyclohexane

General procedure: A 2 mL crimp-top GC vial was charged with NiBr2(DME) (6.2 mg, 0.02 mmol, 0.1 equiv), dppf (11 mg, 0.02 mmol, 0.1 equiv), and activated Zn powder [35] (26.2 mg, 0.4 mmol, 2 equiv). The vial was crimped shut and the olefin (0.2 mmol, 1 equiv) was injected through the septum as a solution in 0.3 mL THF followed by 0.2 mL HFIP. The iodide (1-2 equiv) was then added (as a solution in THF, if solid) and the vial was shaken at 1000 rpm for 12 h at 25 C. The reaction was diluted with EtOAc and quenched by the addition of 1 M HCl (aq). The aqueous phase was extracted with three portionsof EtOAc. The combined organic phase was then passed through a plug of silica. An aliquot of the organic phase was used for GC or GC/MS analysis with mesitylene as an internal standard. Solvent was removed and the mixture was purified by chromatography on silicagel with EtOAc/hexane as the eluent to give the products as colorless oils.

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

Reference:
Article; Diccianni, Justin B.; Chin, Mason; Diao, Tianning; Tetrahedron; vol. 75; 31; (2019); p. 4180 – 4185;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 52548-14-8,Some common heterocyclic compound, 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, molecular formula is C8H7IO2, 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 mixture of 2-iodobenzoic 1a (0.2 mmol), acetylacetone 2a (0.4 mmol), and Cs2CO3 (65.2 mg, 0.20 mmol) in CH3CN was stirred at 100 C. When the reaction was considered complete as determined by TLC analysis, the reaction was allowed to cool to room temperature and quenched by water, and the mixture was extracted with CH2Cl2. The combined organic extracts were washed with water and saturated brine. The organic layers were dried over Na2SO4, filtered. Solvents were evaporated under reduced pressure. The residue was purified by chromatography on silica gel to afford isocoumarins derivatives and isoquinolone derivatives.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Iodo-5-methylbenzoic acid, its application will become more common.

Reference:
Article; Liu, Lei; Hu, Jie; Wang, Xiang-Chuan; Zhong, Mei-Jin; Liu, Xue-Yuan; Yang, Shang-Dong; Liang, Yong-Min; Tetrahedron; vol. 68; 27-28; (2012); p. 5391 – 5395;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 6940-76-7, These common heterocyclic compound, 6940-76-7, name is 1-Chloro-3-iodopropane, 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.

Step 2: 4-Bromo-5-(3-chloro-propyl)-3-methyl-pyrazole-1 -sulfonic acid dimethylamideBrTo a solution of 4-bromo-3-methyl-pyrazole-1 -sulfonic acid dimethylamide (6.7 g, 25 mmol) in diethyl ether (75 ml.) was added dropwise at -780C under N2 phenyl lithium (1.8 M, 14.6 ml_, 26.3 mmol) in dibutyl ether. After warming to O0C for 15 m, the reaction mixture was re-cooled to -780C and a solution of 3-chloro-iodopropane (15.3 g, 75 mmol) in 20 ml. THF was added dropwise. The reaction was warmed to room temperature and stirred for 3 h before quenching with a saturated aqueous solution of NH4CI. The quenched reaction mixture was extracted with EtOAc and the organic layer was dried over Na2SO4, filtered and concentrated. The crude product was purified over normal phase silica starting with 5% EtOAc in heptane for 10 m and then increasing to 50% EtOAc in heptane for 20 m to give the desired product as a clear oil (3.85 g, 1 1.2 mmol) MS m/z 346.3 (M+H)+.

The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; ASTEX THERAPEUTICS LIMITED; HOWARD, Steven; MORTENSON, Paul Neil; HISCOCK, Steven Douglas; WOOLFORD, Alison Jo-Anne; WOODHEAD, Andrew James; CHESSARI, Gianni; O’REILLY, Marc; CONGREVE, Miles Stuart; DAGOSTIN, Claudio; CHO, Young Shin; YANG, Fan; CHEN, Christine Hiu-Tung; BRAIN, Christopher Thomas; LAGU, Bharat; WANG, Yaping; KIM, Sunkyu; GRIALDES, John; LUZZIO, Michael Joseph; PEREZ, Lawrence Blas; WO2010/125402; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 335349-57-0, 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. 335349-57-0, name is 5-Chloro-4-iodo-2-nitroaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example E5 (RS)-5-(2,2-Dimethyl-[1,3]dioxolan-4-ylmethoxy)-4-iodo-2-nitro-phenylamine Prepared from 5-chloro-4-iodo-2-nitro-phenylamine (Example A1) (4.48 g, 15 mmol), D,L-alpha, beta-isopropylidene-glycerol (10 mL, 81 mmol) and KOH (1.01 g, 18 mmol) in DMSO (10 mL) at 23 C. according to the general procedure E. Obtained as a yellow solid (4.9 g). MS (ISN) 393 [(M-H)-]; mp 151 C.

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-Chloro-4-iodo-2-nitroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hoffmann-la Roche Inc.; US6407094; (2002); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com