Month: March 2021

Synthetic Route of 460-37-7,Some common heterocyclic compound, 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, molecular formula is C3H4F3I, 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.

In a tubular reactor, evacuated and replaced twice with nitrogen, and 10 ml of methyl tert-butyl ether solvent was added under a nitrogen atmosphere.1 mmol of the compound of the above formula (II),2mmol of the above formula iodide compound,2.5 mmol of azide trimethylsilane,2mmol tert-butyl peroxybenzoateAnd 0.02 mmol of a copper hexafluorophosphate tetraacetonitrile catalyst is dissolved in the above solvent,The reaction was stirred at a temperature of 30 C for 2 hours. After the reaction was completed, the reaction liquid was cooled to room temperature, filtered, and the solvent was evaporated under reduced pressure.Purification of the compound of formula III by column chromatography,The yield was 92.7%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,1-Trifluoro-3-iodopropane, its application will become more common.

Reference:
Patent; Zhang Haiying; Zhou Lanlan; (12 pag.)CN108440503; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 624-76-0, name is 2-Iodoethanol, 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. Quality Control of 2-Iodoethanol

To a solution of compound 3 (2.00g, 6.43mmol) in acetone (20mL) was added potassium carbonate (1.33g, 9.64mmol), 2-iodoethanol (0.60mL, 7.72mmol) and stirred overnight at room temperature. After completion of the reaction, 120 water (150mL) and ethyl acetate (150mL) were added and the mixture was extracted with ethyl acetate twice. The combined extracts were washed with water (50mL¡Á2) and brine (50mL¡Á2), and dried over Na2SO4. After filtration, the solvent was removed under vacuum to obtain the crude compound. The crude compound was then purified by column chromatography on silica (60% EA/PE) to give compound 24 4 as a yellow oil (2.10g, yield 92.0%). 1H NMR (400MHz, CDCl3) delta 7.35 (s, 5H), 5.51 – 5.47 (m, 1H), 5.30 – 5.26 (m, 1H), 5.24 – 5.12 (m, 2H), 4.60 – 4.54 (m, 1H), 3.69 – 3.63 (m, 2H), 3.02 – 2.90 (m, 2H), 2.68 – 2.64 (m, 2H), 1.43 (s, 9H). 13C NMR (150MHz, CDCl3) delta 170.96, 155.46, 135.12, 128.76, 128.72, 128.62, 80.45, 67.63, 60.76, 53.77, 53.56, 36.29, 34.91, 28.39. ESI-MS: [M+Na]+ m/z 378.2

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

Reference:
Article; Du, Xinming; Qian, Jiawen; Wang, Yujie; Zhang, Mingming; Chu, Yiwei; Li, Yingxia; Bioorganic and Medicinal Chemistry; vol. 27; 13; (2019); p. 2784 – 2800;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 5326-47-6, 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. 5326-47-6, name is 2-Amino-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 2-amino-5-iodobenzoicacid (17) (15 mmol, 4.0 g) in methanol(16 mL) was added concentrated H2SO4 (3.0 mL). Thereaction mixture was refluxed for 6 h and stirred at room temperature for additional12h. After removal of the solvent, the residue was poured into 100 mL saturatedNaHCO3 solution and extracted with ethyl acetate(3¡Á15 mL). The organic layer was separated, washed with brine (3¡Á15 mL), driedover anhydrous Na2SO4, filteredand concentrated to give the product methyl 2-amino-5-iodobenzoate (18) as yellow solid, Yield: 94%, mp:70-73C. 1H NMR (400 MHz, DMSO-d6, ppm) delta: 8.13 (1H,d, J = 2.16 Hz), 7.47 (1H, dd, J = 8.68, 2.16 Hz), 6.45 (1H, d, J = 8.72 Hz), 5.42 (2H, s, NH2),3.86 (3H, s, O-CH3). C8H8INO2.

The synthetic route of 2-Amino-5-iodobenzoic acid has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kang, Dongwei; Zhang, Heng; Zhou, Zhongxia; Huang, Boshi; Naesens, Lieve; Zhan, Peng; Liu, Xinyong; Bioorganic and Medicinal Chemistry Letters; vol. 26; 21; (2016); p. 5182 – 5186;,
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 869500-07-2 as follows. Formula: C7H6BrI

29.7 g of 1-bromo-2-iodo-3-toluene was dissolved in 300 ml of 1,4-dioxane solvent.Stirring under nitrogen, adding 20.2 g of o-bromobenzeneboronic acid,34.5 g of K2CO3, 1.15 g of tetrakis(triphenylphosphine)palladium, and the temperature was raised to reflux.After 5 hours, the basic reaction of the raw materials was determined by HPLC, and the reaction solution was dried under reduced pressure.The residue was subjected to column chromatography to give Intermediate 22-1 as 22.1 g (0.068 mol). (Yield: 81%)

According to the analysis of related databases, 869500-07-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Beijing Lv Ren Science And Technology Co., Ltd.; Lv Yao; Feng Yu; Jia Xueyi; (40 pag.)CN108409773; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 52548-63-7, 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 52548-63-7 as follows.

To a 500 mL round- bottomed flask was added 5-fluoro-2-iodo-benzoic acid (23 g, 86.5 mmol) in methanol (230 mL). To the resulting solution was added cone, sulfuric acid (2.3 mL, 43.2 mmol). The reaction mixture was warmed to 65 oC and stirred for 15 h. The resulting mixture was concentrated under reduced pressure to give crude producte which was then was partitioned between EtOAc (250 mL) and a half sat. Na2CO3(ac?) solution (250 mL). The layers were thoroughly mixed and then separated. The organic layer was dried over magnesium sulfate, filtered, and concentrated under reduced pressure to give a yellow oil (23 g, 95% yield). 1 H NMR (400 MHz, CDCI3): 7.94 (dd, J = 8.7, 5.4 Hz, 1 H), 7.54 (dd, J = 9.0, 3.1 Hz, 1 H), 6.93 (m, 1 H), 3.94 (s, 3H).

According to the analysis of related databases, 52548-63-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; CHAI, Wenying; LETAVIC, Michael, A.; LY, Kiev, S.; PIPPEL, Daniel, J.; RUDOLPH, Dale, A.; SAPPEY, Kathleen, C.; SAVALL, Brad, M.; SHAH, Chandravadan, R.; SHIREMAN, Brock, T.; SOYODE-JOHNSON, Akinola; STOCKING, Emily, M.; SWANSON, Devin, M.; WO2011/50198; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 4387-36-4, name is 2-Iodobenzonitrile, molecular formula is C7H4IN, 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. Quality Control of 2-Iodobenzonitrile

Example VI; tert.butyl[[1-(2-cyano-phenyl)-1H-indol-5-yl]-(3,5-dichloro-phenylsulphonyl)-amino]-acetate; 300 mg tert.butyl[(3,5-dichloro-phenylsulphonyl)-(1H-indol-5-yl)-amino]-acetate, 12 mg copper iodide and 307 mg potassium phosphate are placed in a flask. It is evacuated twice and filled with argon. Then 1 ml of toluene and 166 mg 2-iodo-benzonitrile are added. After the addition of 21 mul N,N’-dimethyl-trans-cyclohexanediamine the mixture is heated to 110¡ã C. for 8 hours. Then it is divided between water and ethyl acetate. The aqueous phase is extracted with ethyl acetate and the combined organic phases are dried on magnesium sulphate. The solvents are eliminated in vacuo and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 10:1 to 1:2).Yield: 266 mg (73percent of theory)Mass spectrum (ESI+): m/z=573 [M+NH4]+

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4387-36-4, its application will become more common.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2010/93703; (2010); 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. 461-17-6, name is 1,1,1-Trifluoro-4-iodobutane, This compound has unique chemical properties. The synthetic route is as follows., Formula: C4H6F3I

250g water, 18.9g (purity 93%, 440mmol) sodium hydroxide, and 95.2g (400mmol) 4,4,4-trifluorobutyliodide were placed in a 500ml four-necked flask equipped with a stirrer, a reflux cooler, and a thermometer. By heating, the mixture was maintained at 90C for 36 hours while being stirred. As the reaction proceeds, generation of gas was observed. Upon completion of the reaction, concentrated hydrochloric acid was added to the reaction mixture and the mixture was extracted 3 times with 200ml chloroform. The results of a gas chromatography analysis performed on the extract and the collected gas indicated that 4,4,4-trifluorobutyliodide was converted at 86.8% conversion rate, and the selectivity for 4,4,4-trifluorobutanol, 4,4,4-trifluoro-1-butene, and bis(4,4,4-trifluorobutyl)ether were 44.9%, 50.2%, and 4.9%, respectively.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 461-17-6.

Reference:
Patent; Tosoh F-Tech, Inc.; EP1403238; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 610-97-9, A common heterocyclic compound, 610-97-9, name is Methyl 2-iodobenzoate, molecular formula is C8H7IO2, 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: A 50 cm3 Schlenk flask was charged with an ortho-substituted iodoarene(1¡Á10-3 mol), an amine (1.1-5¡Á10-3 mol), K2CO3(2¡Á10-3 mol), a catalyst (5¡Á10-6 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¡Á7 cm3 of diethyl ether (3¡Á15 min with stirring) and then GCanalyzed with dodecane as the internal standard (0.076 cm3, 5.46¡Á10-4 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

The synthetic route of 610-97-9 has been constantly updated, and we look forward to future research findings.

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

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 289039-29-8 as follows. Product Details of 289039-29-8

2-chloro-5-iodo-benzamidine 374.8 mL (374.8 mmol) lithium bis-trimethylsilylamide (1 M in hexane) are placed in 300 mL diethyl ether and combined with 50.0 g (189.8 mmol) 2-chloro-5-iodobenzonitrile. The reaction mixture is stirred for 1.5 hours at ambient temperature under an argon atmosphere and then cooled to 0 C. Then 5 molar hydrochloric acid is slowly added. The precipitate thus formed is suction filtered and dried. Yield: 56.0 g

According to the analysis of related databases, 289039-29-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Brandl, Trixi; Maier, Udo; Hoffmann, Matthias; Scheuerer, Stefan; Joergensen, Anne T.; Pautsch, Alexander; Breitfelder, Steffen; Grauert, Matthias; Hoenke, Christoph; Erb, Klaus; Pieper, Michael; Pragst, Ingo; US2007/244104; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 481075-58-5, A common heterocyclic compound, 481075-58-5, name is 2-Bromo-1-iodo-4-(trifluoromethyl)benzene, molecular formula is C7H3BrF3I, 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.

A solution of xantphos (0.277 g, 0.479 mmol), Pd2(dba)3 (0.146 g, 0.160 mmol), 2-bromo-1-iodo-4-(trifluoromethyl)benzene (Oakwood Chemical, 1.232 g, 3.51 mmol), (E)-ethyl 3-(2-amino-5-(benzylthio)phenyl)acrylate (1.000 g, 3.19 mmol), and potassium phosphate (2.032 g, 9.57 mmol) in 10 mL dioxane was heated to 90 C. for 5 hours. The reaction mixture was diluted with water and extracted with DCM. The organics were dried over MgSO4 and concentrated. The crude residue was used in the next step without purification. m/z (ESI) 536.0 (M+H)+.

The synthetic route of 481075-58-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Amgen Inc.; Weiss, Matthew; Boezio, Alessandro; Boezio, Christiane; Butler, John R.; Chu-Moyer, Margaret Yuhua; Dimauro, Erin F.; Dineen, Thomas; Graceffa, Russell; Guzman-Perez, Angel; Huang, Hongbing; Kreiman, Charles; La, Daniel; Marx, Isaac E.; Milgrim, Benjamin Charles; Nguyen, Hanh Nho; Peterson, Emily; Romero, Karina; Sparling, Brian; US9212182; (2015); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com