Month: June 2021

Reference of 364-12-5, 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. 364-12-5, name is 5-Bromo-2-iodobenzotrifluoride, This compound has unique chemical properties. The synthetic route is as follows.

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The chemical industry reduces the impact on the environment during synthesis 5-Bromo-2-iodobenzotrifluoride. I believe this compound will play a more active role in future production and life.

Reference:
Article; Nino, Patricia; Caba, Marta; Aguilar, Nuria; Terricabras, Emma; Albericio, Fernando; Fernandez, Joan-Carles; Indian Journal of Chemistry – Section B Organic and Medicinal Chemistry; vol. 55B; 7; (2016); p. 854 – 881;,
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 444-29-1 as follows. COA of Formula: C7H4F3I

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.

According to the analysis of related databases, 444-29-1, the application of this compound in the production field has become more and more popular.

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

Application of 29289-13-2, 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. 29289-13-2 name is 2-Iodo-4-methylaniline, 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.

General procedure: A mixture of 2-halobenzenamine (1.0 mmol), isothiocyanate (1.2 mmol), Et3N (2.0 mmol) and MCM-41-2N-CuSO4 (0.0025 mmol) in DMSO (2 mL) was stirred under an air atmosphere at 80 C for 5-24 h. After completion of the reaction as indicated by TLC, the mixture was cooled to room temperature. The solution was diluted with ethyl acetate (30 mL ) and filtered. The catalyst was washed with ethyl acetate (2 × 5 mL) and Et2O (2 × 5 mL) and reused in the next run. The organic layer was washed with water (2 × 10 mL) and dried over anhydrous Na2SO4. After evaporating under vacuum, the residue was purified by flash chromatography on silica gel (petroleum/ethyl acetate = 10:1 to 4:1) to provide the corresponding pure product 3.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Iodo-4-methylaniline, and friends who are interested can also refer to it.

Reference:
Article; Xiao, Ruian; Hao, Wenyan; Ai, Jinting; Cai, Ming-Zhong; Journal of Organometallic Chemistry; vol. 705; (2012); p. 44 – 50;,
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. 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 181765-86-6

Add compound 7 (9.99 g, 29.4 mmol) to a 250 ml three-necked flaskAnd p-methoxyphenylboronic acid (5.36g, 35.28mmol),Then add 50ml of tetrahydrofuran and 50ml of water and stir,Add bistriphenylphosphonium palladium dichloride (1.03g, 1.47mmol) under a nitrogen atmosphere.When the temperature reached 60 C, sodium carbonate (6.23g, 58.8mmol) was added, and the reaction was refluxed for 12h.Cooled to room temperature, diluted with ethyl acetate, washed with saturated brine, and dried over anhydrous magnesium sulfate,After filtration, the solution was concentrated under reduced pressure and separated by column chromatography to obtain 7.53 g.Compound 8 was a white solid with a yield of 80%.

The synthetic route of 181765-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Dalian University of Technology; Wang Shisheng; Li Guangzhe; Liu Liqiang; Zhao Weijie; Guo Xiuhan; Li Yueqing; Wang Xu; Dong Huijuan; (21 pag.)CN110041200; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 58755-70-7,Some common heterocyclic compound, 58755-70-7, name is 1-Iodo-4-methoxy-2-nitrobenzene, molecular formula is C7H6INO3, 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.

Example 2 Compound 6 Compound 6 was prepared from compound 5 (3.35 g, 12 mmol), trimethylsilylacetylene (3.3 mL, 24 mmol), PdCI2(PPh3)2 (0.42 g, 5.0 mol %), and CuI (0.114 g, 5.0 mol %) in TEA (70 mL). The reaction mixture was diluted with EtOAC and filtered through a silica gel bed, the organic layer was washed with water, and dried over Na2SO4. The dried organic layer was concentrated and purfied by chromatographic separation using (Hex:AcOEt = 100:10(v/v)) gave 1.66 g (55%) of compound 6.

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-4-methoxy-2-nitrobenzene, its application will become more common.

Reference:
Patent; THRESHOLD PHARMACEUTICALS, INC.; WO2006/57946; (2006); A2;,
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. 3930-83-4, name is 2-Iodobenzamide, A new synthetic method of this compound is introduced below., COA of Formula: C7H6INO

General procedure: A two-neck round bottom flask was charged with amagnetic stirrer, evacuated and backfilled with argon. 2-iodobenzamide ( 0.5mmol, 124 mg), aniline or alpha-substituted benzylamine (1.0 mmol), K2CO3(1.0 mmol, 138 mg) and CuBr2 (0.05mmol, 11 mg) in DMSO (5 mL) under argon atmosphere. The mixture was allowed tostir under argon atmosphere at 110 C for 4 h.The mixture was concentrated with the aid of a rotary evaporator, and theresidue was purified by column chromatography on silica gel using petroleumether/ethyl acetate (2:1) as eluent to provide the product 2-9.

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; Wang, Li-Xia; Hu, Ben-Quan; Xiang, Jun-Feng; Cui, Jie; Hao, Xiang; Liang, Tong-Ling; Tang, Ya-Lin; Tetrahedron; vol. 70; 45; (2014); p. 8588 – 8591;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 1829-28-3,Some common heterocyclic compound, 1829-28-3, name is Ethyl 2-iodobenzoate, molecular formula is C9H9IO2, 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.

Weighing 5.52 g (20 mmol) of o-iodobenzoic acid ethyl ester obtained by esterification of o-iodobenzoic acid with anhydrous ethanol in a microwave reaction tube, 1.08 g (10 mmol) of o-phenylenediamine.Add copper iodide (190 mg, 1 mmol) in turn,Potassium phosphate (6.36g, 30mmol),Appropriate amount of ethylene glycol and magnetron at 180 C,Microwave reaction under nitrogen protection,The reaction was stopped after 1 h, and the reaction was terminated by TLC. Extraction with ethyl acetate (3 x 100 mL),Wash with water and an appropriate amount of saturated brine, combine the organic layers, add anhydrous Na2SO4 to remove water,After filtration, the residue was concentrated and the residue was purified by column chromatography to yield 1.The yield of the obtained Compound 1 was 65%.

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

Reference:
Patent; Xinxiang Medical University; Yan Fulin; Cao Ke; Yan Jianwei; Ma Lijuan; Lv Haixia; Wang Yawen; Yin Tiantian; (25 pag.)CN108586364; (2018); A;,
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. 387-48-4, name is 3-Fluoro-2-iodobenzoic acid, A new synthetic method of this compound is introduced below., SDS of cas: 387-48-4

Step B: Preparation of Ethyl 2-(3-fluoro-2-iodophcnyl)acctate; 109081 A solution of 3-fluoro-2-iodobenzoic acid ( 14.90 g, 56.0 mmol) was stirred in thionyl chloride ( 150 mL) for 1 hour at reflux. The mixture was cooled to room temperature, and the excess thionyl chloride was removed in vacuo to give the corresponding acid chloride. HbO (20 ml.) was added, and a solution of TMSCHN? (2.0M in Ht2O. I I O mL. 220 mmol) was added. The mixture was stirred for 4 hours, and the excess reagent was quenched by the addition of AcOH. The mixture was then partitioned between EtOAc (200 mL) and saturated NaHCO3 solution. The layers were separated, and the organic layer was washed twice with saturated NaHCO3, once with water, and once with brine once. The organic layer was then dried over anhydrous MgStheta4 and concentrated in vacuo. This material was dissolved in HtOH (200 proof) and silver(I)oxide (2.60 g, 1 1 .2 mmol) was added. The suspension was heated to 800C for 30 minutes, cooled to room temperature, and filtered through celite. The filtrate was concentrated in vacuo, and the resulting oil was purified by flash chromatography to give 9.90 g of product as a yellow oil.

The synthetic route of 387-48-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AMGEN INC.; WO2008/76427; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 610-97-9, 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. 610-97-9 name is Methyl 2-iodobenzoate, 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.

General procedure: A 50 cm3 Schlenk flask was charged with an ortho-substituted iodoarene(1×10-3 mol), an amine (1.1-5×10-3 mol), K2CO3(2×10-3 mol), a catalyst (5×10-6 mol), and a stirring bar. Next, 5cm3 of DMF was added. Under balloon pressure of CO, the reactionmixture was stirred at 100 C for 1-6 h. After the reaction, the Schlenkflask was cooled down, and the organic products were extracted with3×7 cm3 of diethyl ether (3×15 min with stirring) and then GCanalyzed with dodecane as the internal standard (0.076 cm3, 5.46×10-4 mol). Each reaction was repeated minimum twice and the averagevalue from two experiments was reported. The difference between tworesults was below 5%.After the solvents were evaporated, the crude product was purifiedby flash chromatography on silica gel using hexane/ethyl acetate (10:4)as the eluent, and the corresponding N-substituted phthalimides wereobtained

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

Reference:
Article; Wojcik, Przemys?aw; Trzeciak, Anna M.; Applied Catalysis A: General; vol. 560; (2018); p. 73 – 83;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 4387-36-4, 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. 4387-36-4, name is 2-Iodobenzonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Weigh 0.6 mM halogenated aromatic hydrocarbon in a reaction flask, add 4 mL of solvent, and fill the reaction flask with nitrogen.Deoxygenation was performed for 30 minutes and 150 muL of triethylamine and 24 mM pyrrole or its derivatives were sequentially added during the deoxygenation. After that, the reaction vessel was sealed, placed over a light-emitting diode (LED) having a wavelength of 450 nm and a power of 30 W to be irradiated, and the reaction was stirred at room temperature for 20 hours.After the end of the reaction, the light source was switched off and the reaction mixture was spin-dried. Column chromatography was performed using petroleum ether and ethyl acetate as eluents. After vacuum drying at 35° C., the carbon-carbon coupling product 6a was obtained. The nuclear magnetic resonance spectrum of compound 6a was obtained. As shown in FIG. 34 and FIG. 35 , the nuclear magnetic carbon spectrum shows that the yield of compound 6a is 96percent, as shown in Table 1. The halogenated aromatic hydrocarbon is o-iodobenzeneacetonitrile and the solvent is acetonitrile.When the pyrrole in Example 16 was replaced with N-methylpyrrole, a carbon-carbon coupling product 6b was obtained. The nuclear magnetic and nuclear magnetic carbon spectra of compound 6b were as shown in FIGS. 36 and 37, and the yield of compound 6b was 96percent, as shown in Table 1. When the pyrrole in Example 16 is replaced with N-phenylpyrrole, a carbon-carbon coupling product 6c is obtained. The nuclear magnetic and nuclear magnetic carbon spectra of compound 6c are shown in Figs. 38 and 39, and the yield of compound 6c is: 58percent, as shown in Table 1.

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; Shaanxi Normal University; Fang Yu; Miao Rong; (29 pag.)CN108002991; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com