Month: May 2021

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 7212-28-4 as follows. Recommanded Product: 2-Iodo-N-phenylacetamide

General procedure: 0.3 g (1.56 mmol) of 7, 1.87 mmol of 3a-j and 0.32 g (2.34 mmol) of K2CO3 were combined and refluxed in 20 ml of acetone for 2 h. The solvent was evaporated under reduced pressure and the crude product was washed with water, filterred and dried. The pure product was obtained by recrystallization from petroleum ether and ethyl acetate.

According to the analysis of related databases, 7212-28-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Wukun; Hua, Jie; Zhou, Jinpei; Zhang, Huibin; Zhu, Haiyang; Cheng, Yanhua; Gust, Ronald; Bioorganic and Medicinal Chemistry Letters; vol. 22; 15; (2012); p. 5008 – 5012;,
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. 203626-41-9, name is 1-Chloro-2-iodo-3-(trifluoromethyl)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C7H3ClF3I

Reference Production Example 31; To 9 ml of 1,4-dioxane was added 1.5 g of 2-iodo-3-chlorobenzo trifluoride, 1. 62 g of potassium carbonate, 0.17 g of tetrakis(triphenylphosphinepalladium) and 0.72 g of 4-pyridineboronic acid, and the mixture was stirred at 90C for 4 hours and at 120C for 10 hours. Thereafter, the resultant reaction mixture was poured into a saturated ammonium chloride aqueous solution, and the mixture was extracted with ethyl acetate three times. The organic layers obtained by extraction were combined and washed with saturated saline, dried over anhydrous magnesium sulfate, then, concentrated. The resultant residue was subjected to silica gel column chromatography to obtain 0.5 g of 4-(2-chloro-6-trifluoromethylphenyl)pyridine. [Show Image] 1H-NMR:7.18(d 2H),7.49(t,1H),7.69-7.73(m,2H),8.71(d,2H)

The synthetic route of 203626-41-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sumitomo Chemical Company, Limited; EP2332936; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 239135-53-6, name is 2-Fluoro-4-iodo-1-(trifluoromethyl)benzene, 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. Recommanded Product: 239135-53-6

Intermediate 79: 3,4-bis(Benzyloxy)-6-[(E)-2-[3-fluoro-4-(trifluoromethyI)- phenyl]ethenyl]pyridazine A vessel containing 3,4-bis(benzyloxy)-6-ethenylpyridazine (Intermediate 78, 1.09 g, 3.42 mmol), tris-(2-methylphenyl)phosphane (0.208 g, 0.685 mmol), 2-f.uoro-4-iodo-l- (trifluoromethyl)benzene (1.191 g, 4.1 1 mmol) and palladium(II) acetate (0.038 g, 0.171 mmol) was evacuated and acetonitrile (10 ml) and triethylamine (9.07 ml, 65.1 mmol) were added in vacuo and then the mixture was flushed with nitrogen. The reaction was then heated in the microwave at 80 C for 4 hours and, upon cooling, was diluted with dichloromethane and washed with saturated aqueous ammonium chloride solution. The organics were dried ( gSC^), filtered and solvent removed in vacuo to give a brown oil which was purified by column chromatography (silica, eluting with 30- 100 % dichloromethane in petrol) to yield 3,4-bis(benzyloxy)-6-[(E)-2-[3-fiuoro-4- (trifluoromethyl)phenyl]ethenyl]pyridazine (1.1 g, 2.29 mmol, 67 % yield). 1H NMR (CDCI3) delta 7.53 – 7.68 (m, 3 H), 7.31 – 7.53 (m, 12 H), 6.97 (s, 1 H), 5.71 (s, 2 H) and 5.28 (s, 2 H). MS ES+: 481.

The synthetic route of 2-Fluoro-4-iodo-1-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; FARNABY, William; FIELDHOUSE, Charlotte; HAZEL, Katherine; KERR, Catrina; KINSELLA, Natasha; LIVERMORE, David; MERCHANT, Kevin; MILLER, David; WO2013/27000; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 1032231-24-5, name is 2-Bromo-5-iodobenzaldehyde, This compound has unique chemical properties. The synthetic route is as follows., Safety of 2-Bromo-5-iodobenzaldehyde

Step 2: (2-bromo-5-iodophenyl)methanolTo a solution of 2-bromo-5-iodobenzaldehyde (12.4 g, 40 mmol) in MeOH (50 mL) was added NaBH4 (3 g, 80 mmol) at 0 C. After the addition, the reaction solution was stirred at rt for 30 minutes. The reaction solution was diluted with water (20 mL) and EtOAc (60 mL). The organic layer was separated and dried over anhydrous Na2S04. After removal of solvent, the residue was purified with column chromatography to afford (2-bromo-5- iodophenyl)methanol (3.5 g, 1 1 .2 mmol, 28 % yield) as a white solid.

According to the analysis of related databases, 1032231-24-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GLAXO GROUP LIMITED; JOHNS, Brian Alvin; SHOTWELL, John Brad; HAIGH, David; WO2012/67663; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 268568-11-2, name is Ethyl 2-amino-5-iodobenzoate, 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 268568-11-2, Recommanded Product: 268568-11-2

General procedure: As a typical experiment, the reaction of 4-(trifluoromethyl)bromobenzene (0.225 g, 1 mmol), methyl 3-amino-4-methylthiophene-2-carboxylate (0.342 g, 2 mmol) and KOAc (0.196 g, 2 mmol) at 120 C during 20 h in DMAc (3 mL) in the presence of PdCl(C3H5)(dppb) (12.2 mg, 0.02 mmol) under argon affords methyl 3-amino-4-methyl-5-(4-trifluoromethylphenyl)-thiophene-2-carboxylate 1a after extraction with dichloromethane, evaporation and filtration on silica gel (pentane/ether) in 82% (0.258 g) yield.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Derridj, Fazia; Si Larbi, Karima; Roger, Julien; Djebbar, Safia; Doucet, Henri; Tetrahedron; vol. 68; 36; (2012); p. 7463 – 7471;,
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. 845866-78-6, name is 1-Bromo-3-iodo-5-(trifluoromethoxy)benzene, A new synthetic method of this compound is introduced below., COA of Formula: C7H3BrF3IO

Example A51 a) Preparation of intermediate Chloro-difluoro-acetic acid methyl ester (1.38 mL, 13.082 mmol) was added to a stirred mixture of l-bromo-3-iodo-5-trifluoromethoxybenzene (2 g, 5.451 mmol), potassium fluoride (380 mg, 6.541 mmol) and copper iodide (1.38 g, 6.541 mmol) in DMF (20 mL) in a sealed tube and under N2 atmosphere. The mixture was stirred at 120 C for 18 h, then it was diluted with water and extracted with Et20. The organic layer was separated, dried over MgSC^, filtered and the solvents evaporated in vacuo. The crude product was purified by flash column chromatography (silica; pentane). The desired fractions were collected and concentrated in vacuo (200 mbar) to yield a colourless oil (1.41 g, 83%, volatile compound).

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; JANSSEN PHARMACEUTICALS, INC.; ROMBOUTS, Frederik, Jan, Rita; TRABANCO-SUAREZ, Andres, Avelino; GIJSEN, Henricus, Jacobus, Maria; MACDONALD, Gregor, James; BISCHOFF, Francois Paul; ALONSO-de DIEGO, Sergio-Alvar; VELTER, Adriana, Ingrid; VAN ROOSBROECK, Yves, Emiel, Maria; WO2013/171712; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 1000802-34-5, 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 1000802-34-5 as follows.

To a solution of 6-iodobenzo[d][1,3]dioxol-5-amine (1 g, 3.8 mmol) and paraformaldehyde (1.14 g, 38 mmol) in methanol (10 mL) was added NaBH3CN (2.39 g, 38 mmol) slowly with stirring. The mixture was heated to 50 C. for 4 h. Water (100 mL) was added and extracted with methylene chloride (100 mL). The organic layer was washed with brine (100 mL), dried (MgSO4) and evaporated under vacuum to give crude title compound 0102-15 (1.16 g) as a brown oil which was used directly to the next step without further purification. LCMS: 292 [M+1]+; 1H NMR (DMSO-d6) delta 2.56 (s, 6H), 6.02 (s, 2H), 6.96 (s, 1H), 7.32 (s, 1H).

According to the analysis of related databases, 1000802-34-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Curis, Inc.; Cai, Xiong; Qian, Changgeng; (62 pag.)US2016/317508; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 1483-73-4, 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. 1483-73-4 name is Diphenyliodonium bromide, 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.

EXAMPLE 34 Preparation of trans-3-phenyl-4-(4-phenoxyphenyl)-2-piperidone 34 6.2 g (0.023 mol) of trans-4-(4-hydroxyphenyl)-3-phenyl-2-piperidone 27, 8.6 g (0.023 mol) of diphenyliodonium bromide and a solution of 0.94 g of sodium hydroxide in 170 cm3 of double-distilled water are brought to reflux with stirring for 24 hours. The mixture is cooled and extracted with methylene chloride. The organic phase is washed successively with 5% strength sodium hydroxide solution and with water to neutrality, and dried over anhydrous sodium sulfate. After filtration and evaporation, 6 g of a solid are obtained and this is recrystallized in methanol. 5.3 g (66%) of pure 34 are obtained, m.p. 157-159 C. Analysis: C23 H21 NO2: IR(KBr): nuN–H at 3,200 cm-1, moderate, nuC=O at 1,660 cm-1, strong, nuC–O–C at 1,240 cm-1, strong.

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

Reference:
Patent; Laboratoires Hoechst S.A.; US4785007; (1988); A;,
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 1252046-13-1 as follows. COA of Formula: C7H3BrIN

Add bromo-(2-ethoxy-2-oxo-ethyl)zinc (2.97 g, 12.7 mmol) (prepared according to Example 9A) to a mixture of 2-bromo-5-iodo-benzonitrile (2.60 g, 8.44 mmol), bis(dibenzylideneacetone)palladium (0.121 g, 0.211 mmol) and 4,5-bis(diphenylphosphino )5 9,9-dimethylxanthene (0.122 g, 0.211 mmol) in THF (20 mL), then the reaction mixture is stirred at 65 C for 1 h under nitrogen. The reaction mixture is quenched with water (10 mL). The result mixture is extracted with EtOAc (10 mL x 3). The combined organic phases are washed with water (1 0 mL ), concentrated to afford a black residue, which is purified by column chromatography on silica gel eluting with PE:EtOAc (20: 1) to afford the title 10 compound (1.00 g, 42.0% Yield) as a yellow solid. 1H NMR (400MHz, CD3Cl) 8 = 7.65 (d, J = 8.4 Hz, 1H), 7.60 (d, J = 2.0 Hz, 1H), 7.39 (dd, J = 2.0, 8.4 Hz, 1H), 4.18 (q, J = 7.2 Hz, 2H), 3.61 (s, 2H), 1.28 (t, J = 7.2 Hz, 3H)

According to the analysis of related databases, 1252046-13-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ELI LILLY AND COMPANY; LILLY CHINA RESEARCH AND DEVELOPMENT CO., LTD.; MA, Tianwei; WU, Liang; ZHANG, Xuejun; (109 pag.)WO2019/41340; (2019); 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. 141738-80-9, name is 3-Chloro-4-iodobenzotrifluoride, A new synthetic method of this compound is introduced below., SDS of cas: 141738-80-9

A. (2-Chloro-4-trifluoromethylphenyl)-acetic Acid A solution of LiHMDS in toluene was prepared by the addition of n-BuLi (357 mL of a 1.6 M solution in hexanes, 571 mmol) to a cold (-78 C.) solution of HMDS (120.5 mL, 571 mmol) in toluene (700 mL). After 30 min, the reaction mixture was allowed to warm up to 10 C. over 1 h. The solution was then transferred via a cannula to a flame-dried, three-neck flask under N2 containing Pd2 dba3 (4.18 g, 4.57 mmol) and (2′-dicyclohexylphosphanylbiphenyl-2-yl)-dimethylamine (3.77 g, 9.59 mmol). The mixture was stirred for 15 min at 15 C., cooled to -10 C. and t-butylacetate (70.5 mL, 525.4 mmol) was added dropwise. After 10 min, 3-chloro-4-iodobenzotrifluoride (70 g, 228.4 mmol) was added and the reaction mixture was warmed up to 28 C. After stirring at this temperature for 1.5 h, the mixture was filtered through silica gel, using toluene as eluent, and the solvent was removed in vacuo. The residue was purified using flash chromatography (silica gel, 98:2 hexanes:EtOAc) to yield (2-chloro-4-trifluoromethylphenyl)-acetic acid tert-butyl ester as a solid.

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; Renaud, Johanne; Missbach, Martin; McKie, Jeffrey A.; Bhagwat, Shripad S.; US2004/92572; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com