Month: July 2021

Related Products of 328-73-4,Some common heterocyclic compound, 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, molecular formula is C8H3F6I, 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.

The compound represented by the formula (1d) was synthesized by the following method.First, in the four-necked flask purged with argon by the following procedure,3,5-dibromo-2-cyclohexyloxythiophene[Document description: K.K. Morimitsu, K.M. Shibata, S. Kobatake, M.M. Irie, J.M. Org. Chem. , 67, 4574-4578 002)] 1.2 g (3.4 mmol)Dissolve in 60 mL of anhydrous tetrahydrofuran,Cooled to -80 C. 1.6 M n-butyllithium hexane solution 2.4 mL (3.8 mmol) was slowly added dropwise,Stir for 1 hour. Next, tributyl borate 1.1 mL(4.1 mmol) was slowly added dropwise and stirred for 1 hour.Add water to stop the reaction, return to room temperature,3,5-bis (trifluoromethyl) iodobenzene 1.2 g (3.4 mmol), Pd (PPh3) 4 80 mg,Add 6.0 mL of 20 wt% sodium carbonate aqueous solution,The set temperature of the oil bath was 80 C. and refluxed for 7 hours.After returning to room temperature, neutralize with dilute hydrochloric acid,Extracted with diethyl ether.After washing the organic layer with saturated aqueous sodium chloride solution,Add magnesium sulfate and dry,The magnesium sulfate was removed by filtration and concentrated.Then, it isolate | separates by silica gel column chromatography (Rf = 0.3) using hexane as a developing solvent, and HPLC.(Developing solvent: hexane)Yield 1.1g, Yield 66%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Iodo-3,5-bis(trifluoromethyl)benzene, its application will become more common.

Reference:
Patent; Osaka City University; Obata, Makoto; (25 pag.)JP2019/151632; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 6828-35-9, These common heterocyclic compound, 6828-35-9, name is 5-Chloro-2-iodoaniline, 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: 2-Iodoaniline 2a (65.7 mg, 0.3 mmol), Cu(OAc)2 (6 mg, 10%), KOtBu (101 mg, 0.9 mmol), DMAc (1.0 mL) were mixed in a Schlenck tube and then to the mixture was added 2-(phenylethynyl)benzonitrile1a (74 mg, 0.36 mmol) under N2. The reaction mixture was stirred for 12 h at 120 C under N2. After the reaction was completed (monitored by TLC), the reaction mixture was then diluted with water and extracted with ethyl acetate. After the combined organic layers were washed with brine, dried over Na2SO4, and concentrated under reduced pressure, the residue was purified by flash column chromatography on silica gel using petroleum ether/ethyl acetate as eluent to afford the pure product 3

The synthetic route of 6828-35-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Liu, Xiaodong; Deng, Guobo; Liang, Yun; Tetrahedron Letters; vol. 59; 29; (2018); p. 2844 – 2847;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

42861-71-2, name is 3-Iodophenyl acetate, 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: 3-Iodophenyl acetate

Step 1: 3-{(6-[4-(2-Trifluoromethylbenzoyl)piperazin-l-yl]pyridazin-3-yl)ethynyl}- phenyl acetate: Prepared by Sonogashira coupling reaction of Intermediate 6 with 3-iodophenyl acetate in a mixture of triethylamine and DMSO to give the product as an off-white solid; IR (KBr) 2926, 2216, 1640, 1434, 1316, 1116, 1010, 785 cm”1; 1H NMR (300 MHz, CDCl3) delta 2.31 (s, 3H), 3.29-3.86 (m, 2H), 3.70-4.10 (m, 6H), 6.90 (d, J= 9.9 Hz, IH), 7.11 (d, J= 7.2 Hz, IH), 7.32-7.76 (m, 8H); ESI-MS (m/z) 454.88 (M)+.

The synthetic route of 42861-71-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; WO2008/62276; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 4387-36-4, name is 2-Iodobenzonitrile, 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 4387-36-4, Formula: C7H4IN

0.25 mmol of 2-cyanoiodobenzene, 0 l of the cyanide reagent K4 [Fe (CN) 6] was added to a 25 mL screw test tube, Sodium acetate 0.25 mmol, 100 mg 3 wtpercent Pd / Ce ?, and then 7 mL of N, N-dimethylformamide and lmL isopropanol Organic solvent to test tube, 500W visible light irradiation under the magnetic stirring reaction, control visible light intensity of 0.74W / cm2, anti Should be the temperature of 65 ° C, 10 hours after the reaction to stop the reaction, take a small amount of reaction solution by microporous membrane filtration, methanol solvent dilution And the liquid sample to be tested, the sample to be tested with 2-cyanide iodobenzene standard, phthalonitrile standard for high-performance liquid phase detection comparison The selectivity of the reaction product was 94.1percent, the selectivity of the target product was 49.7percent, and the liquid product yield was 46.8percent. Rear Processing method for the use of cloth funnel filter washing catalyst, drying for recycling use; reaction solution by dichloromethane and water After the mixed solution was extracted, the organic layer was concentrated and the final product phthalonitrile was obtained by column chromatography. The isolated yield was 42percent

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

Reference:
Patent; Nanjing University of Technology; Guo, Cheng; Gong, Xubin; Wu, Lou; Li, Qing; Wang, Jianjiang; (11 pag.)CN105777579; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 64248-58-4,Some common heterocyclic compound, 64248-58-4, name is 1,2-Difluoro-4-iodobenzene, molecular formula is C6H3F2I, 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 mixture of methyl indole-5-carboxylate 7a (2 g, 11.4 mmol), 1-iodo-3,4-difluoro-benzene 8a (1.5 mL, 12.5 mmol), CuI (0.22 g, 1.14 mmol), trans-N,N’-dimethylcyclohexane-1,2-diamine (0.54 mL, 3.43 mmol), and K3PO4 (6.06 g, 28.5 mmol) in toluene (12 mL) was heated at 110 C. for 7 h. The reaction mixture was diluted with CH2Cl2 and filtered. The solution was concentrated and the residue was purified by flash column chromatography (silica gel, 20% EtOAc/heptane) to give 3.0 g of compound 8b. MS m/z 288.1 (M+H+).

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

Reference:
Patent; Connolly, Peter J.; Bian, Haiyan; Li, Xun; Liu, Li; Macielag, Mark J.; McDonnell, Mark E.; US2013/102584; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 455-13-0, name is 4-Iodobenzotrifluoride, 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 455-13-0, COA of Formula: C7H4F3I

General procedure: In a typical experiment, the isolated crystalline precatalyst 1A (or 2A, 0.005 mmol) was sequentially mixed with 3 mL of solvent (DMF or [Bmim]PF6 if required), iodobenzene (5mmol), phenylacetylene (6 mmol), and Et3N (7.5 mmol). The obtained mixture was placed in a sealed Teflon-lined stainless steel autoclave, purged with syngas (CO, 1.0 MPa) and then stirred vigorously at the required temperature for the appointed time. Upon completion of the reaction, the mixture wasc ooled to room temperature and the pressure was carefully released. The reaction mixture was extracted with diethyl ether(5 mL 3). The ether fractions were combined and then analyzedby GC to determine the conversion of PhI (1-dodecane as an internal standard) and the selectivity for the carbonylative products (normalization method). The structures of the carbonylative products were further confirmed by GC-MS.

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

Reference:
Article; Yang, Da; Wang, Dongliang; Liu, Huan; Zhao, Xiaoli; Lu, Yong; Lai, Shijun; Liu, Ye; Cuihua Xuebao/Chinese Journal of Catalysis; vol. 37; 3; (2016); p. 405 – 411;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 4387-36-4, The chemical industry reduces the impact on the environment during synthesis 4387-36-4, name is 2-Iodobenzonitrile, I believe this compound will play a more active role in future production and life.

2-{[(4alphaS)-l-(4-Fluorophenyl)-5-hydroxy-4alpha-methyl-l,4,4alpha,5,6,7-hexahydrocyclopenta[fJindazol-5- yl]ethynyl}benzonitrile (20-1). Disopropylamine (0.052 mL, 0.364 mmol) was added to a solution of 1-6 (112 mg, 0.363 mmol), 2-iodobenzonitrile (113 mg, 0.401 mmol), bis(triphenylphosphine)palladium30 (II) chloride (5.10 mg, 0.008 mmol), and CuI (1.38 mg, 0.008 mmol) in anhydrous THF (1.0 mL) at ambient temperature. The resulting solution was stirred at ambient temperature for 2.0 hours, then diluted with diethyl ether, filtered through a pad of celite and the solvent removed in vacuo. Purification by flash chromatography on 40 g of silica, eluting with a gradient of 0-90percent EtOAc in hexanes afforded 50 mg, 33 percent of 20-1 as a yellow foamy solid. MS (ESI): m/z = 410.2 (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, 2-Iodobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK & CO., INC.; WO2008/51532; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 146137-72-6, name is 2-Fluoro-6-iodobenzaldehyde, 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 146137-72-6, category: iodides-buliding-blocks

General procedure: Acetyl phenyl boronic acid derivatives (3.78 g, 20.77 mmol) were reacted with halogen containing aldehyde partners (4 g, 16 mmol) or alternatively, aldehyde phenyl boronic acid starting materials (3.9 g, 21.13 mmol) were reacted with halogen substituted acetophenones (4.0 g, 16.25 mmol) for the Suzuki coupling reaction. Thus, aryl halide and polymer bound Pd (PPh3)4 (0.25 g, 1.35 mol%) were added to a dioxane-ethanol (30 mL, 4:1) mixture. This was followed by the addition of triethylamine (1.17 mL, 32 mmol) and the boronic acid derivative. The resultant solution was degassed several times with argon and stirred in ice or refluxed for 6-48 h depending upon the starting materials used. After the reaction, the mixture was filtered through celite and evaporated to dryness. The crude material was purified by column chromatography (10-20% ethyl acetate/ hexane) to obtain pure intermediates 5a-5h.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Fluoro-6-iodobenzaldehyde, and friends who are interested can also refer to it.

Reference:
Article; Sharma, Horrick; Sanchez, Tino W.; Neamati, Nouri; Detorio, Mervi; Schinazi, Raymond F.; Cheng, Xiaolin; Buolamwini, John K.; Bioorganic and Medicinal Chemistry Letters; vol. 23; 22; (2013); p. 6146 – 6151;,
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. 20691-72-9, name is 4-Iodo-2-nitroaniline, A new synthetic method of this compound is introduced below., Product Details of 20691-72-9

To a stirred solution of SnC¾ (78.0 g, 346 mmol) in concentrated HC1 (150 mL) was added 2 (25.4 g, 92.0 mmol) in three portions over 30 min at rt. The reaction mixture was heated at 70 C for 1 h and then stirred at 0 C overnight. The mixture was treated with ¾0 (150 mL) and stirred for 2 h. The precipitate was collected by filtration and dried under vacuum to afford 3 (17 g, 81% yield) as a grey solid. LC-MS (ESI) m/z 235.0 (M + H)+.

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; PRESIDIO PHARMACEUTICALS, INC.; LI, Leping; ZHONG, Min; WO2011/150243; (2011); A1;,
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.

Compound 5.3. Methyl 3-iodo-4-methylbenzoate. To a solution of 3-iodo-4- methylbenzoic acid (28.0 g, 0.107 mol) in MeOH (300 mL) at 0 C was carefully added concentrated H2SO4 (30 mL). The mixture was heated at 60 C overnight, then cooled and the solvent removed under reduced pressure. The residue was carefully poured onto ice- water (200 mL) and the mixture was extracted with EtOAc (500 mL). The organics was washed with water (100 mL), saturated NaHC03 (100 mL), brine (100 mL), dried (MgS04), filtered, and concentrated to yield the title compound as a brown oi 1 (29.0 g, 98%). ‘H NMR (400 MHz, CDCI3) delta 8.47 (d, J = 1 .7 Hz, 1 H), 7.90 (dd, J = 7.9 Hz, 1.7 Hz, 1 H), 7.29 (d, J= 7.9 Hz , 1 H), 3.90 (s, 2H), 2.48 (s, 3H).

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; 3-V BIOSCIENCES, INC.; OSLOB, Johan D.; MCDOWELL, Robert S.; JOHNSON, Russell; YANG, Hanbiao; EVANCHIK, Marc; ZAHARIA, Cristiana A.; CAI, Haiying; HU, Lily W.; WO2014/8197; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com