Month: December 2020

Adding a certain compound to certain chemical reactions, such as: 62720-29-0, name is 1,3-Dibromo-5-fluoro-2-iodobenzene, 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 62720-29-0, Application In Synthesis of 1,3-Dibromo-5-fluoro-2-iodobenzene

Example 101a 2,6-Dibromo-4-fluorobenzaldehyde 101a A solution of 1,3-dibromo-5-fluoro-2-iodobenzene (50 g, 132 mmol) in anhydrous toluene (300 mL) was cooled to -35 C. A solution of isopropylmagnesium chloride (84 mL, 171 mmol, 2.0 M in diethyl ether) over a period of 30 minutes while maintaining the internal temperature below -25 C. See . A clear brown solution was obtained. Stirring was continued for 1.5 h. Then anhydrous DMF (34 mL, 436 mmol) was added over a period of 30 minutes. The temperature of the reaction mixture increased to -19 C. The reaction mixture was warmed to 10 C. (room temperature) over 1 h and stirred at this temperature for 1.5 h. The reaction was quenched with saturated aqueous NH4Cl (100 mL), filtered and evaporated under reduced pressure. The residue was purified by silica-gel column chromatography (eluting with petroleum ether/ethyl acetate:from 50:1 to 20:1) to give 101a (20 g, yield 54%) as a yellow solid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3-Dibromo-5-fluoro-2-iodobenzene, and friends who are interested can also refer to it.

Reference:
Patent; GENENTECH, INC.; Crawford, James John; Young, Wendy B.; US2013/116245; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 387-48-4, name is 3-Fluoro-2-iodobenzoic acid, 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 387-48-4, HPLC of Formula: C7H4FIO2

Intermediate 93: 3-Fluoro-2-(1 H-pyrazol-1 -yl)benzoic acid.3-Fluoro-2-(1 H-pyrazol-1 -yl)benzoic acid. To a mixture of 3-fluoro-2- iodobenzoic acid (1 .4 g, 5.26 mmol), 1 H-pyrazole (0.72 g, 10.5 mmol), trans- N,N’-dimethyl-cyclohexane-1 ,2-diamine (0.17 mL, 1 .05 mmol), Cul (50.1 mg, 0.26 mmol), dioxane (50 mL) and water (0.028 mL) was added Cs2C03 (3.43 g, 10.5 mmol). The reaction mixture was heated to 100 C for 1 h. The reaction mixture was cooled to ambient temperature then diluted with water. The aqueous layer was acidified to pH2 and extracted with EtOAc (30 mL) three times. The organic layers were combined, dried over Na2S04, filtered and concentrated. Purification (FCC), (DCM to 10% MeOH/1 %HOAC/DCM) afforded the title compound as a colorless oil (790 mg, 72%). 1H NMR (400 MHz, CDCIs): 7.85 – 7.73 (m, 1 H), 7.54 – 7.44 (m, 1 H), 7.44 – 7.34 (m, 1 H), 6.55 (s, 1 H).

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-Fluoro-2-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; LETAVIC, Michael; RUDOLPH, Dale, A.; SAVALL, Brad, M.; SHIREMAN, Brock, T.; SWANSON, Devin; WO2012/145581; (2012); A1;,
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. 852569-38-1, name is 5-Chloro-4-fluoro-2-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C6H4ClFIN

Potassium t-butoxide (12.52 g, 111.6 mmol) is added at room temperature to a solution of 5-chloro-4-fluoro-2-iodoaniline (5.0 g, 22.3 mmol) in 250 mL of anhydrous THF under nitrogen. After stirring for 15 minutes, a solution of 1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carboxylic acid fluoride (5.67 g, 24.6 mmol) in 30 mL of anhydrous THF is added dropwise. The reaction mixture is stirred for 4 hours at room temperature and then poured into saturated aqueous NaHCO3 solution and extracted with EtOAc. The organic phase is washed with saturated aqueous NaCl solution, dried over Na2SO4 and concentrated to dryness. After purification by flash chromatography on silica (cyclohexene/EtOAc:95/5 to 80/20), a red solid is obtained, which is purified by flash chromatography on amine phase (DCM) to give 2.84 g of a white solid (yield: 31%). [0871] LCMS (Method E): MH+=404.0, RT=2.29 min

The synthetic route of 852569-38-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SANOFI; Benazet, Alexandre; Duclos, Olivier; Guillo, Nathalie; Lassalle, Gilbert; Macary, Karim; Vin, Valerie; US2014/235616; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 628-77-3, name is 1,5-Diiodopentane, 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 628-77-3, Application In Synthesis of 1,5-Diiodopentane

Intermediate 3 was prepared by a similar procedure from intermediate 1 (500 mg, 1.1 mmol), 1 ,5-diiodopentane (1.1 g, 0.5 ml, 3.3 mmol), 1 M aqueous sodium hydroxide (3 ml, 3 mmol), tetra-n-butylammonium iodide (45 mg, 0.12 mmol) and water (3 ml). Purification was achieved via column chromatography (loaded onto diatomaceous earth) using 0-14% step gradient of EtOAc in cyclohexane (2% steps ) as eluent, followed by EPO 100% cyclohexane, followed by 30% EtOAc in cyclohexane to afford the product as a colorless gum.Yield: 324 mg (46%)LC-MS (Method 3): Rt 4.79 min, m/z 642 [MH+]

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, 1,5-Diiodopentane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ARGENTA DISCOVERY LTD.; WO2007/42815; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 18698-96-9, 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. 18698-96-9, name is 2-(2-Iodophenyl)acetic acid, This compound has unique chemical properties. The synthetic route is as follows.

Key Intermediate 1: 2-(2-Ethynylphenyl)butanamide (KI)(a) 2-(2-Iodophenyl)butanoic acid (Ii)Lithium diisopropylamide solution (2.0 M in THF/heptane/ethylbenzene, 3.82 mL, 7.63 mmol) was added to dry THF (10 mL) under an atmosphere of nitrogen and cooled to 0 00. A solution of 2-(2-iodophenyl)acetic acid (500 mg, 1.91 mmol) in dryTHF (15 mL) was then added dropwise. This solution was stirred for 40 minutes at 000 before the addition of iodoethane (0.92 mL, 11 mmol). The solution was returnedto room temperature and stirred for 4 hours. The resulting mixture was quenched with the addition of H20 (10 mL) and then 2 M HCI (20 mL). The aqueous layer was extracted with EtOAc (3 x 30 mL), the organic layers were combined and washedwith brine, dried over Mg504 and the solvent was evaporated under reducedpressure. The residue was adsorbed onto silica gel and purified using columnchromatography (Biotage Isolera, 5i02 cartridge, 0-40percent EtOAc in petroleum benzine40-60 00) to give the title compound Ii as a pale yellow oil (479 mg, 87percent); 1H NMR(400 MHz, d6-DMSO) O 12.49 (5, 1H), 7.88 (dd, J= 7.9, 1.2 Hz, 1H), 7.39 (td, J= 7.6,1.2 Hz, 1H), 7.32 (dd, J= 7.8, 1.7 Hz, 1H), 7.01 (Jm, 1H), 3.77 (t, J= 7.5 Hz, 1H),1.98?1.86 (m, 1H), 1.73?1.60 (m, 1H), 0.85 (t, J= 7.3 Hz, 3H).JH2Ii 12 13 Ki

The chemical industry reduces the impact on the environment during synthesis 2-(2-Iodophenyl)acetic acid. I believe this compound will play a more active role in future production and life.

Reference:
Patent; CANCER THERAPEUTICS CRC PTY LIMITED; FOITZIK, Richard Charles; MORROW, Benjamin Joseph; HEMLEY, Catherine Fae; LUNNISS, Gillian Elizabeth; CAMERINO, Michelle Ang; GANAME, Danny; STUPPLE, Paul Anthony; LESSENE, Romina; KERSTEN, Wilhelmus Johannes Antonius; HARVEY, Andrew John; HOLMES, Ian Peter; WO2014/26243; (2014); 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. 610-97-9, name is Methyl 2-iodobenzoate, A new synthetic method of this compound is introduced below., Computed Properties of C8H7IO2

30 g (114 mmol) methyl 2-iodobenzoate, N, N-dimethylformamide in 1 L round bottom flaskAfter adding 360ml, trimethylsilylacetylene 22.5g (229mmol), 114.9 ml (801 mmol) triethylamineNitrogen was bubbled for 20 minutes by addition of 8 g (11 mmol) of dichloro (bistriphenylphosphine) palladium (II),I put 2.2 g (11 mmol) of Cooper (I) iodideHeat stirred at 80 C. for 3 h.When the reaction was terminated, the reaction solution was purified by a column to obtain 23 g (yield: 86%) of the compound represented by [Formula 191-d].

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; SFC Ltd.; Park Seok-bae; Lee Se-jin; Kim Jeong-su; (92 pag.)KR101996647; (2019); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 82777-09-1,Some common heterocyclic compound, 82777-09-1, name is 2′-Iodo-1,1′:3′,1”-terphenyl, molecular formula is C18H13I, 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: The outline of our synthetic routes to the 6 compounds listed in Fig. 1 is shown in Scheme 1. They were synthesized by Suzuki-Miyaura coupling of 2,6-dibromodithieno[3,2-b:2?,3?-d]thiophene each with the corresponding boronic acid. Compounds 5 and 7 in Fig. 1 were also synthesized by Suzuki-Miyaura coupling of 3,7-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)dibenzo[b,d]thiophene and 2,6-bis(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)dithieno[3,2-b:2?,3?-d]thiophene with 2?-iodo-1,1?:3?,1?-terphenyl, respectively. The typical procedure is following. A mixture of 2,6-dibromo-dithieno[3,2-b:2?,3?-d]thiophene (174.0 mg, 0.5 mmol), boronic acid of counterpart (1.5 mmol), tetrakis (triphenylphosphine) palladium (81.5 mg, 0.08 mmol) and Cs2CO3 (2.0 mL, 2.0 M in aqueous) in 8 mL solvent of toluene: THF = 1:1 was stirred at reflux temperature for 8 h. All reactions were carried out under nitrogen atmosphere with anhydrous solvents. The mixture was poured into water (30 mL) and extracted with CH2Cl2 (20 mL ¡Á 3). The combined extract was washed with brine (40 mL), dried (Na2SO4), and concentrated in vacuo. Column chromatography on silica gel eluted with CHCl3:toluene = 1:1. All compounds were characterized by 1H and 13C NMR and mass spectroscopy.

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-1,1′:3′,1”-terphenyl, its application will become more common.

Reference:
Article; Okada, Shinjiro; Yamada, Kenji; Journal of Molecular Structure; vol. 1037; (2013); p. 256 – 263;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 175278-00-9, 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. 175278-00-9, name is 1-Iodo-2-(trifluoromethoxy)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: For example, synthesis of 1,2-diphenylethyne, 3a. To an oven-dried 5 mL microwave vessel was added Pd(PPh3)2Cl2 (3.5 mg, 0.005 mmol, 2 mol %) and CuI (1.9 mg, 0.01 mmol, 4 mol %). The vessel was then capped and purged with N2 before addition of Cyrene (0.5 mL, 0.5 M), Et3N (38 muL, 0.275 mmol, 1.1 equiv), iodobenzene (27.9 muL, 0.25 mmol, 1 equiv), and phenylacetylene (28.8 muL, 0.263 mmol, 1.05 equiv). The reaction mixture was heated to 30 C and maintained at this temperature with stirring for 1 h before the vessel was vented, and decapped. The solution was then diluted with EtOAc (10 mL), and washed with water (2¡Á 20 mL) and brine (2 ¡Á 20 mL). The organics were then passed through a hydrophobic frit and concentrated under reduced pressure to give a yellow oil, which was purified by flash chromatography (silica gel, 0-5% Et2O in petroleum ether) to afford the title compound as a white solid (44.5 mg, quant.).

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-(trifluoromethoxy)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Wilson, Kirsty L.; Kennedy, Alan R.; Murray, Jane; Greatrex, Ben; Jamieson, Craig; Watson, Allan J. B.; Beilstein Journal of Organic Chemistry; vol. 12; (2016); p. 2005 – 2011;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 156150-67-3, 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. 156150-67-3, name is 2-Chloro-1-fluoro-4-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: An oven-dried Schlenk tube, containing a Teflon-coated magnetic stir bar was charged with CsF (228 mg, 1.5 mmol, 3 equiv) and bispinacolatodiboron (254 mg, 1 mmol, 2 equiv). Under an argon atmosphere, freshly distilled DMSO (0.4 mL), the appropriate aryl iodide (0.5mmol), and pyridine (0.4 to 1 equiv) were added successively. The reaction mixture was heated to 105 C and stirred for 2 h under argon.

The chemical industry reduces the impact on the environment during synthesis 2-Chloro-1-fluoro-4-iodobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Article; Pinet, Sandra; Liautard, Virginie; Debiais, Megane; Pucheault, Mathieu; Synthesis; vol. 49; 21; (2017); p. 4759 – 4768;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 2401-21-0, 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 2401-21-0 as follows.

(f) Synthesis of p-Nitrobenzyl (5R,6S)-6-[(R)-1-Hydroxyethyl]-2-Chloro-2-Ethanesulfinyl-1-Carbapenam-3-Carboxylate (Compound S15) STR39 Under a dry atmosphere, to a dichloromethane (4 ml) solution of Compound S14 (59 mg, 0.15 mmol) were added water (0.014 ml, 0.78 mmol) and pyridine (0.036 ml, 0.45 mmol), and further added dropwise a dichloromethane (2 ml) solution of iodobenzene dichloride (103 mg, 0.37 mmol) under ice-cooling, and the mixture was stirred at the same temperature for 30 minutes. Subsequently, triethylamine (0.042 ml, 0.30 mmol) was added and the mixture was stirred for 10 minutes. The reaction mixture was diluted with ethyl acetate, washed with an aqueous 5percent citric acid solution and water. The aqueous layer was reverse-extracted with ethyl acetate. The ethyl acetate solutions were combined, washed with an aqueous NaCl-saturated solution and dried. The solvent was removed by distillation under reduced pressure. The residue was purified by a medium pressure silica gel column chromatography (Lobar size A, ethyl acetate-hexane 3:2–>1:0) to obtain a mixture (pale yellowish viscous material, 51 mg, 77percent) of some isomers of Compound S15.

According to the analysis of related databases, 2401-21-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Ajinomoto Co., Inc.; US5342963; (1994); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com