Month: September 2021

Adding a certain compound to certain chemical reactions, such as: 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, 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 112671-42-8, Safety of 4-Bromo-1-iodo-2-nitrobenzene

4-bromo-l-iodo-2-nitrobenzene (3 g, 9.18 mmol) was dissolved in anhydrous THF (20 mL) under N2 atmosphere, and the flask was cooled to -78 C. The mixture was stirred for 5 minutes and n-BuLi (4.4 mL, 2.5mol/L) was slowly added. The reaction mixture turned dark and stirring was continued at -78C for 15 minutes. Then, compound OA-1 (1.92 g, 11 mmol) was slowly added to the mixture. The reaction was stirred for 30 minutes at-78 C and then warmed to room temperature. The mixture was poured into water (50 mL) and extracted with CH2CI2 (2 x 20 mL). The organic phases were separated and washed with brine, dried over Na2S04 and concentrated to dryness. The resulting residue was purified by silica gel column chromatography (eluent: petroleum ether/ ethyl acetate = 3/1), resulting in compound OA-2 (1.3 g, 38 % yield). Method A2; Rt: 1.04 min. m/z=: 378.7 (M+H)+ Exact mass: 378.0

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-1-iodo-2-nitrobenzene, and friends who are interested can also refer to it.

Reference:
Patent; JANSSEN R&D IRELAND; VANDYCK, Koen; VERSCHUEREN, Wim, Gaston; RABOISSON, Pierre, Jean-Marie, Bernard; WO2013/98313; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 19094-56-5, These common heterocyclic compound, 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, 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.

To a dried flask, 5-iodo-2-chlorobenzoic acid (20.0 g, 70.8 mmol) and dichloromethane (60 mL) were added. The reaction mixture was stirred, then oxalyl chloride (9.8 g, 77.9 mmol) and DMF (0.2 mL) were slowly added dropwise, and some bubbles were observed. The reaction mixture was stirred at room temperature for 7 hours. The solvent and excess oxalyl chloride were removed by rotary evaporation to give a gray solid, which was used directly in the next step without further purification.

The synthetic route of 19094-56-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangsu Hansoh Pharmaceutical Co., Ltd.; ZHONG, Huijuan; LIAO, Jianchun; YU, Hongping; XU, Yaochang; LI, Qing; CHEN, Jianghua; GAO, Peng; TAN, Songliang; WANG, Shaobao; (45 pag.)US2016/222047; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 31827-94-8, 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. 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: Carbothioamide 2 (0.396 g, 2.0 mmol) was added to a stirredsolution of 2-bromo-1-(4-fluorophenyl)ethanone (0.434g, 2.0 mmol) in absolute ethyl alcohol (25 ml). The reactionmixture was stirred at room temperature for 20 h. Next, thereaction mixture was added to water (50 ml) and neutralizedwith NaHCO3 solution. The product was extracted withdichloromethane (2 × 50 ml), the solvent was evaporated invacuo, and the solid was washed with diethyl ether to affordthe desired product to yield 0.27 g (43%)

The synthetic route of 2-Bromo-1-(4-iodophenyl)ethanone has been constantly updated, and we look forward to future research findings.

Reference:
Article; ??czkowski, Krzysztof Z.; Landowska, Katarzyna; Biernasiuk, Anna; Sa?at, Kinga; Furga?a, Anna; Plech, Tomasz; Malm, Anna; Medicinal Chemistry Research; vol. 26; 9; (2017); p. 2088 – 2104;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 355-43-1, 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. 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: In a Pyrex glass tube were placed olefin (0.2 mmol), perfluoroalkyl iodide (1.0 mmol), and CH2Cl2 (5 mL). Then Na2S2O3 (0.5 mmol, 79 mg) and water (1 mL) were added to the mixture. After sealing the tube, the mixture was shaked and then irradiated with a Hg lamp at room temperature. After the reaction was completed, the mixture was extracted with CH2Cl2. The extract was washed with brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography to afford pure product.

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, 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Yajima, Tomoko; Jahan, Ishrat; Tonoi, Takayuki; Shinmen, Manami; Nishikawa, Aya; Yamaguchi, Kanako; Sekine, Izumi; Nagano, Hajime; Tetrahedron; vol. 68; 34; (2012); p. 6856 – 6861;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 31827-94-8, name is 2-Bromo-1-(4-iodophenyl)ethanone, molecular formula is C8H6BrIO, 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. category: iodides-buliding-blocks

General procedure: Thiosemicarbazone 3 (0.317 g, 1.0 mmoles) was added to astirred solution of 2-bromo-1-(4-fluorophenyl)ethanone(0.217 g, 1.0 mmole) in DMF/EtOH (3: 2) (50 ml). Thereaction mixture was stirred under room temperature for 2 h,and separate precipitate was collected by filtration, suspendedin water and neutralized with NaHCO3 solution.The crude product was purified on silica gel column chromatography(230-400 mesh) using (dichloromethane/methanol, 80:20, Rf = 0.74) to afford the desired product:0.38 g, 87%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 31827-94-8, its application will become more common.

Reference:
Article; ??czkowski, Krzysztof Z.; Anusiak, Joanna; ?witalska, Marta; Dzitko, Katarzyna; Cytarska, Joanna; Baranowska-??czkowska, Angelika; Plech, Tomasz; Paneth, Agata; Wietrzyk, Joanna; Bia?czyk, Joanna; Medicinal Chemistry Research; vol. 27; 4; (2018); p. 1131 – 1148;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 450412-29-0, These common heterocyclic compound, 450412-29-0, name is 1-Bromo-3-fluoro-2-iodobenzene, 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.

Step 2. 6-Bromo-2-fluoro-3′-methylbiphenyl: Pd(Ph3P)4 in a 500-mL round- bottom flask under N2 atmosphere was treated sequentially with a solution of 1- bromo-3-fluoro-2-iodo-benzene (30 g, 0.1 mol) in toluene (250 mL), a solution of 2N aq Na2CO3 (200 mL) and 3-methyl phenylboronic acid in ethanol (62 mL). This mixture was heated at reflux under N2 for 12 h, then cooled to rt. The mixture was partitioned between water and EtOAc. The combined organic layers were washed with brine, dried over MgSO4, evaporated and purified by column chromatography to give 6-bromo-2-fluoro-3′-methyl-biphenyl (12 g). 1H NMR (400MHz, CD3OD): 7.03 (m, 2H), 7.48-7.04 (m, 4H), 7.50 (d, IH).

The synthetic route of 450412-29-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; VITAE PHARMACEUTICALS, INC.; WO2008/124582; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

19094-56-5, A common compound: 19094-56-5, name is 2-Chloro-5-iodobenzoic acid, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

General procedure: To a stirred suspension of 2-chloro-5-iodobenzoic acid(5.65 g, 0.02 mol) in CH2Cl2(20 mL) was added oxalylchloride(1.80 mL, 0.021 mol) and DMF(0.02 mL). Theresulting mixture was stirred for 4 h at room temperature.The mixture was concentrated, and the residual colorlesssolid was dissolved in CH2Cl2(40 mL). To this solutionwere added corresponding substituted benzene(0.02 mol)and then AlCl3(2.75 g, 0.021 mol) portionwise so that thetemperature did not exceed 0 °C. After being stirred at 10?20 °C for 3 h, the mixture was poured into ice water andextracted with CH2Cl2 three times. The combined organiclayers were washed with 1M HCl, water, and brine, thendried over MgSO4 and concentrated. The residual solid wascrystallized from ethanol to give as white solid.According to this procedure the following compoundswere prepared. (2-chloro-5-iodophenyl)(4-fluorophenyl)methanone (1a)White solid, yield 92percent, m.p. 69?70 °C. 1H NMR (400MHz,DMSO-d6): delta 7.38?7.40(m, 2H), 7.41(d, J=8.0 Hz, 1H), 7.82(dd, J=2.4 Hz, 8.0 Hz, 2H), 7.90(d, J=2.4 Hz, 1H), 7.92?7.95(m, 1H). 13C NMR (100MHz, DMSO-d6): delta 116.19,129.47, 131.65, 132.1, 132.65, 136.78, 139.69, 140.20,164.54, 166.56, 191.36. HRMS (ESI) m/z (pos):382.91890C13H7ClFIONa [M+Na]+(calcd. 382.91118).

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-Chloro-5-iodobenzoic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Hu, Shengquan; Sun, Wuji; Wang, Yeming; Yan, Hong; Medicinal Chemistry Research; vol. 28; 4; (2019); p. 465 – 472;,
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 34683-73-3 as follows. HPLC of Formula: C6H12ClI

(6) Synthesis of 15-chloro-3,6,9-trioxapentadecyl azide NaH (54.7 mg, 2.28 mmol), 2-(2-(2-azidoethoxy)ethoxy)ethanol (160.3 mg, 0.915 mmol), and THF (3 mL) were added to a 30-mL eggplant flask, followed by 2 hours of stirring at room temperature under an argon atmosphere. 1-chloro-6-iodohexane (152 muL, 1.01 mmol) was added to the solution, followed by 3.5 hours of stirring. Since the raw materials remained on TLC, 1-chloro-6-iodohexane (28 muL, 0.183 mmol) was added and then the solution was further stirred for 16 hours. Since the raw materials still remained, NaH (11.2 mg, 0.467 mmol) was added and then the solution was stirred for 5.5 hours. However, TLC remained unchanged. H2O was added to quench the reaction, and then the solvent was removed under reduced pressure. CHCl3 and 1M HCl were added to the flask and then the solution was stirred. The organic layer was collected and dried with MgSO4, and then the solvent was removed under reduced pressure. The thus obtained product was purified by flash column chromatography (elution solvent: hexane/EtOAc=6/1), and thus 42.6 mg (0.145 mmol, 15.8% yield) of a target product was obtained.

According to the analysis of related databases, 34683-73-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Toho University; FURUTA, Toshiaki; SONE, Masaki; SUZUKI, Akinobu; OKA, Eri; US2014/256015; (2014); 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. 624-75-9, name is 2-Iodoacetonitrile, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C2H2IN

Compound 6 (prepared according to B2. b) (30 mg) was dissolved in 20 ml of MECN, and iodo acetonitrile (1.0 eq. ) and K2CO3 (3 eq, 29 mg) were added. Stirring for 17 days at 20C. The MECN was evaporated and the residue was purified by preparative TLC using CHCL2/MEOH (9/1) as the eluent. Yield: compound 60 (52 %).

According to the analysis of related databases, 624-75-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; ARTS, Frank, Xavier, Jozef, Herwig; WO2005/28479; (2005); A2;,
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, Computed Properties of C5H10I2

Synthesis of Compound 59.1 [0424] To a solution of tert-butyl 2-(hydroxymethyl)pyrrolidine-l -carboxylate (1.0 g, 4.9 mmol, 1.0 eq) in MeCN (50 mL) were added NaOH (0.39 g, 9.8 mmol, 2.0 eq) and 1, 5- diiodopentane (3.2 g, 9.9 mmol, 2.0 eq). The reaction mixture was stirred at room temperature for 48 h and concentrated under reduced pressure. The residue was diluted with ethyl acetate (100 mL), washed with H20 (100 mL) and brine (50 mL). The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column (PE : EA = 5 : 1) to give 59.1 (0.7 g, Y: 36%) as a yellow oil. 1H NMR (400 MHz, CDC13) delta: 3.96-3.92 (m, 1H), 3.54-3.51 (m, 1H), 3.48-3.39 (m, 2H), 3.33-3.32 (m, 3H), 3.19 (t, J = 6.8 Hz, 2H), 2.31-2.19 (m, 1H), 1.95-1.76 (m, 6H), 1.60-1.50 (m, 3H), 1.46 (s, 9H).

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; BIOGEN IDEC MA INC.; JENKINS, Tracy; VESSELS, Jeffery; WO2014/143672; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com