Tag: M.W=200-300

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 618-91-7 as follows. HPLC of Formula: C8H7IO2

To the mixture of methyl 3-iodobenzoate (157 mg, 0.60 mmol), potassium carbonate (166 mg, 1.20 mmol), cupper(I) iodide (14 mg, 0.07 mmol) and PdCi2(Ph3P)2 (21 mg, 0.03 mmol) in tetrahydrofuran (2 mL) was added tert-butyl propiolate (330 muL, 2.40 mmol) at room temperature. After stirred for 20 h at 60C, the mixture was evaporated to dryness. The residue was chromatographed on a silica gel (EtOAc:hexanes 0: 1~1 : 10) to give the title compound 9-1 (155 mg, 99% yield) as a light brown oil. 1H NMR (300 MHz, CDCl3) delta 8.25 (t, J= 1.4, 1H), 8.16 – 8.05 (m, 1H), 7.80 – 7.68 (m, 1H), 7.46 (t, J= 7.8, 1H), 3.93 (s, 3H), 1.55 (s, 9H).

According to the analysis of related databases, 618-91-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; THE BROAD INSTITUTE, INC.; MASSACHUSETTS GENERAL HOSPITAL; HUNG, Deborah; STANLEY, Sarah; KAWATE, Tomohiko; IWASE, Noriakie; SHIMIZU, Motohisa; WO2013/49567; (2013); A1;,
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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. 51628-12-7, name is 2-(4-Iodophenyl)acetonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C8H6IN

To a solution of 4-iodophenylacetonitrile (6.88 g, 28.3 mmol, 1 eq.) and bis-(2-chloro-ethyl)-carbamic acid tert-butyl ester (7.2 g, 30 mmol, 1.05 eq.) in DMSO (100 mL) under argon (Ar) was added NaNH2 (2.46 g, 60 mmol, 2 eq.) in portions over 15 min. The reaction was stirred at room temperature for 0.5 h, then poured onto ice (200 g), diluted with EtOAc (250 mL) and stirred for 1 h. The organic layer was separated and the aqueous layer was washed repeatedly with EtOAc until colorless. The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated by rotary evaporation to afford an orange oil which was purified by flash column chromatography by eluding with 7-12% EtOAc/hexanes to yield 4-cyano-4-(4-iodo-phenyl)-piperidine-1-carboxylic acid tert-butyl ester as a pale orange oil/solid (8.28 g, 18.96 mmol, 67%). 1H NMR (300 MHz, CDCl3): delta 7.82 (dd, 2H), 7.26 (dd, 2H), 4.38 (br. s, 2H), 4.28 (br. t, 2H), 2.15 (m, 2H), 2.0 (td, 2H), 1.59 (s, 9H).

The synthetic route of 51628-12-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PHARMACOPEIA, INC.; US2003/13720; (2003); A1;,
Iodide – Wikipedia,
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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. 128140-82-9, name is 1-(Difluoromethoxy)-4-iodobenzene, A new synthetic method of this compound is introduced below., SDS of cas: 128140-82-9

A mixture of 1-(difluoromethoxy)-4-iodobenzene (1.35 g, 5.00 mmol, 1.00 equiv), 4,4,5,5- tetramethyl-2-(tetramethyl- 1,3 ,2-dioxaborolan-2-yl)- 1 ,3,2-dioxaborolane (1.413 g, 5.56 mmol, 1.10 equiv), AcOK (1.47 g, 14.98 mmol, 3.00 equiv), and Pd(dppf)C12 (186 mg, 0.25 mmol, 0.05 equiv) in dioxane (30 mL)/ water(3 mL) was stirred for 2 h at 95C under nitrogen. The mixture was diluted with water and extracted with ethyl acetate. The combined extracts were washed with brine, dried over anhydrous sodium sulfate, and concentrated under vacuum. The residue was purified by a silica gel column eluting with ethyl acetate/petroleum ether (1:50) to afford the title compound (660 mg, 49%) as colorless oil.

The synthetic route of 128140-82-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; CHEN, Huifen; CHU, Yanyan; DO, Steven; ESTRADA, Anthony; HU, Baihua; KOLESNIKOV, Aleksandr; LIN, Xingyu; LYSSIKATOS, Joseph P.; SHORE, Daniel; VERMA, Vishal; WANG, Lan; WU, Guosheng; YUEN, Po-wai; WO2015/52264; (2015); A1;,
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Adding a certain compound to certain chemical reactions, such as: 19099-54-8, name is 1-Iodo-2-isopropylbenzene, 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 19099-54-8, name: 1-Iodo-2-isopropylbenzene

0.3 mmol of sodium carbonate and 0.1 mmol of 1,2-bis(4-methoxyphenyl)acetylene,Tetrakis(triphenylphosphine palladium) 0.005 mmol, bis(2-diphenylphosphinophenyl)ether 0.005 mmol,0.2 mmol of (4-(methylthio)phenyl)boronic acid, 0.3 mmol of 2-isopropyliodobenzene, and 1 mL of N,N-dimethylformamide were added to a 15 mL reaction tube.Nitrogen was repeatedly filled 10 times, placed in an oil bath at 120 C, and reacted for 24 hours;Cooled to room temperature, the reaction was diluted with ethyl acetate, washed with water three times, the organic phase dried over anhydrous Na2SO4, filtered, and concentratedPurification by thin layer chromatography to give 39.4mg of the desired product, yield 82%.

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

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (20 pag.)CN109879713; (2019); A;,
Iodide – Wikipedia,
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Related Products of 103962-05-6, 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. 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of compound 03-1-3 (2.50 g, 7.52 mmol, 1.0 eq), 1-iodo-4- (trifluoromethoxy)benzene (3.25 g, 11.3 mmol, 1.5 eq), CuI (143.2 mg, 752.1 mumol, 0.1 eq), (1S,2S)-N1,N2-dimethylcyclohexane-1,2-diamine (321.0 mg, 2.26 mmol, 0.3 eq) and K3PO4 (3.19 g, 15.0 mmol, 2.0 eq) in toluene (3.0 mL) was heated at 110 °C for 12 h under N2. The reaction mixture was diluted with H2O (100 mL) and extracted with ethyl acetate (80 mL*4). The combined organic layers were washed with brine (20 mL*3), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to give a residue. The residue was purified by column chromatography (SiO2) to give compound 03-1-4 (3.00 g, 74percent). M+H+ = 393.2 (LCMS).

The chemical industry reduces the impact on the environment during synthesis 1-Iodo-4-(trifluoromethoxy)benzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; KYRAS THERAPEUTICS, INC.; VACCA, Joseph P.; LI, Dansu; (587 pag.)WO2017/96045; (2017); A1;,
Iodide – Wikipedia,
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Related Products of 13329-40-3, 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. 13329-40-3, name is 1-(4-Iodophenyl)ethanone belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example QC-13a To a solution of 4-iodophenyl ethanone (14.76 g, 60.0 mmol) in 150 mL of dichloromethane was added bromine (9.5 g, 59.5 mmol) dropwise. The resulting solution was stirred at room temperature overnight. The solvent was removed under vacuum. The crude product was recrystallized with dichloromethane/hexanes to give Example QC-13a (11.8 g, 60.5%) as a grey solid. 1H NMR (500 MHz, CDCl3) delta ppm 4.38 (s, 2H) 7.68 (d, J=8.55 Hz, 2H) 7.86 (d, J=8.85 Hz, 2H); LC/MS: Anal. Calcd. for C8H771BrIO [M+H]+ 325.86; found 325.11.

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-(4-Iodophenyl)ethanone, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bristol-Myers Squibb Company; US2010/249190; (2010); A1;,
Iodide – Wikipedia,
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Some common heterocyclic compound, 51628-12-7, name is 2-(4-Iodophenyl)acetonitrile, molecular formula is C8H6IN, 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. COA of Formula: C8H6IN

iodophenyl cyanide(10 mmol, 2.28 g), Na2C03 (0.5 mmol, 57 mg)Soluble in tetrahydrofuran / water(Nu: nu = 3: 1) in a mixed solvent,After the reaction was stopped for 6 hours, the reaction was stopped. After allowing to stand at room temperature, the solvent was dried and usedSilica gel column chromatography to obtain a white solid after purification of p-iodobenzamide 2. 2 g (Yield: 89%);

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 51628-12-7, its application will become more common.

Reference:
Patent; Suzhou University of Science and Technology; ZHOU, YUYANG; WANG, XIAOMEI; YE, CHANGQING; ZHU, SAIJIANG; XU, PENGJIE; LIANG, ZUOQIN; (6 pag.)CN104016913; (2016); B;,
Iodide – Wikipedia,
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Application of 6940-76-7, 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. 6940-76-7, name is 1-Chloro-3-iodopropane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of (+)-(2S,5R)-1-allyl-2,5-dimethylpiperazine (10.6 g, 68.7 mmol, prepared according to the literature procedure described by Janetka, J.W. et al., J. Org. Chem., 2003, 68, 3976-3980), 1 -chloro-3-iodo-propane (16.9 g, 82.8 mmol, 1.2 eq), and K2CO3 (24.6 g, 178 mmol, 2.6 eq) in acetone (230 mL) was heated at 5O0C for 16 hours. The mixture was cooled to room temperature, filtered through Celite, and the filtrate was concentrated in vacuo. Chromatography on silica gel using a gradient of 2M NHs/MeOH in CH2CI2 (0-2%) gave 14.05 g (89%) of (2S,5fi)-1 -allyl^^S-chloro-propyO^.delta- dimethyl-piperazine as a light yellow oil.To a solution of (2S,5/^-1-allyl-4-(3-chloro-propyl)-2,5-dimethyl-piperazine (14.05 g, 61 mmol) in anhydrous THF (78 mL) under argon was added thiosalicylic acid (10.33 g, 67 mmol, 1.1 eq) followed by the addition of a solution of tris(dibenzylidenacetone)-dipalladium (Pd2(dba)3, 2.8 g, 3.1 mmol, 5 mol%) and1 ,4-bis(diphenylphosphino)butane (DPPB, 1.33 g, 3.1 mmol, 5 mol%) in anhydrous THF (26 mL, pre-mixed for 15 minutes). After stirring at room temperature for 2 hours, the mixture was filtered through Celite. The filtrate was concentrated in vacuo and the residue was partitioned between 1 N aqueous HCI (70 mL) and Et2O (70 mL). The aqueous layer was separated and extracted with Et2O (50 mL x 2), and treated with NaOH (solid) to bring its pH to 13. The aqueous phase was extracted with CHCI3 (50 mL x 4). The combined organic phase was dried (Na2SO4) and concentrated in vacuo EPO to give 11.6 g (100%) of (2S,5/:?)-4-(3-chloro-propyl)-2I5-ciimethyl-piperazine as a light yellow oil.To a solution of (2S,5R)-4-(3-chloro-propyl)-2,5-dimethyl-piperazine (11.6 g, 61 mmol) in CH2CI2 (240 ml_) at O0C was added Boc2O (14.9 g, 67 mmol, 1.1 eq) and the mixture was stirred at room temperature for 16 hours. The solvent was evaporated and the residue was chromatographed on silica gel by eluting with 30% EtOAc/hexane to give 12.8 g (72%) of (2S,5fl)-4-(3-chloro-propyl)- 2,5-dimethyl-piperazine-1-carboxylic acid tert-butyl ester as a light yellow oil. 1H NMR (300 MHz, CDCI3): delta 4.22 (m, 1 H), 3.64 (m, 3H), 3.23 (dd, J = 11.4, 3.9 Hz, 1 H), 2.55 (m, 1 H), 2.42 (m, 1 H), 2.22 (d, J = 11.4 Hz, 1 H), 1.87 (t, J = 6.3 Hz, 2H), 1.46 (s, 9H)7 1.21 (d, J = 6.9 Hz, 3H), 0.92 (d, J = 6.6 Hz, 3H).

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

Reference:
Patent; PHARMACOPEIA DRUG DISCOVERY, INC.; WO2006/44293; (2006); A2;,
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 25309-64-2 as follows. Application In Synthesis of 1-Ethyl-4-iodobenzene

General procedure: To a round-bottom flask were charged with an N?-Boc-N-aryl hydrazine 7 or 14 (48 mmol), 4-substituent iodobenzene 8 (40 mmol), CuI (0.78 g, 4 mmol), 1,10-phenanthroline (1.44 g, 8 mmol), Cs2CO3 (15.64 g, 48 mmol) and 40 mL of dry DMF at room temperature. The reaction mixture was degassed, charged with N2 gas and heated to 80 C. After 4-5 h, the resulting mixture was cooled to room temperature, diluted with ethyl acetate (100 mL), filtered. The filtrate was then washed twice with brine (2×100 mL). The organic layer was dried over anhydrous magnesium sulfate, filtered, concentrated under reduced pressure, The residue was purified by flash chromatography with a mixture of petroleum ether and ethyl acetate as an eluent to afford the desired product, which was recrystallized from a mixture of petroleum ether and ethyl acetate to give the desired crystals 9 or 15.

According to the analysis of related databases, 25309-64-2, the application of this compound in the production field has become more and more popular.

Reference:
Article; Yang, Zhanhui; Hou, Shili; He, Wei; Cheng, Baoxiang; Jiao, Peng; Xu, Jiaxi; Tetrahedron; vol. 72; 17; (2016); p. 2186 – 2195;,
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. 56404-21-8, name is 1-Iodo-2,4-dimethyl-3-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows., Formula: C8H8INO2

Step 2: To a hot suspension of iron powder (2.3 g, 8.3 mmol), ammonium chloride (2.16 g, 38.7 mmol) and water (18 ml.) in ethanol (50 ml.) was added 1-iodo-2,4- dimethyl-3-nitrobenzene in portions over a period of 10 minutes. The resulting mixture was heated at reflux for 1 hour, and filtered hot through a pad of Celite. The Celite was washed with ethanol and ethyl acetate and the filtrate was concentrated in vacuo. The residue was extracted with dichloromethane, the organics were dried over anhydrous sodium sulfate and filtered and the filtrate was evaporated to yield 2.Og (98%) of 3-iodo-2,6-dimethyl- phenylamine as a white solid. MS: 248.1 [M+H]+

According to the analysis of related databases, 56404-21-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; WYETH; WO2009/108838; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com