Category: iodides-buliding-blocks

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

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

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. 25252-00-0, name is 2-Bromo-5-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 25252-00-0

Step I: To a stirred solution of 2-bromo-5-iodobenzoic acid (150 g, 458 mmol) in dichloromethane (1500 ml) was added DMF (2.0 ml) followed by oxalylchloride (58.2 ml, 688 mmol) at 0 C in drop wise fashion over the period of 30 min. After complete addition, the reaction mixture was stirred at room temperature for 3h. Volatiles were evaporated under reduced pressure to give 2-bromo-5-iodo-benzoyl chloride (-158 g). The crude product was used for the next step immediately. (Note: The product should not be exposed to air).

According to the analysis of related databases, 25252-00-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NOVARTIS AG; BEBERNITZ, Gregory Raymond; BOCK, Mark Gary; WO2012/140596; (2012); 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. 328-73-4, name is 1-Iodo-3,5-bis(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., category: iodides-buliding-blocks

General procedure: Sulfuric acid (400?800 muL) was added to a stirred mixture of iodoarene (1 mmol), Oxone (1 mmol, 617 mg) and arene (1.1?3 mmol) in acetonitrile (2 mL). The reaction mixture was stirred overnight and a solution of KBr (2 mmol, 240 mg) in water (10 mL) was added. After the formation of a solid or oily residue, acetonitrile was removed under reduced pressure. To the residue Et2O (10 mL) was added and the suspension stirred for 10 min. The precipitated diaryliodonium bromide was filtrated and washed with water (15 mL) and Et2O (15 mL). The product was dried under vacuo.

The synthetic route of 328-73-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Soldatova, Natalia; Postnikov, Pavel; Kukurina, Olga; Zhdankin, Viktor V.; Yoshimura, Akira; Wirth, Thomas; Yusubov, Mekhman S.; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 849 – 855;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, 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. Safety of 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one

Example 3: Preparation of 3-{3-[(3,4-dimethoxy-bicyclo[4.2.0]octa-l,3,5-trien-7- ylmethyl)-methyl-amino]-propyl}-7,8-dimethoxy-l,3-dihydro-benzo[d]azepin-2- one (Formula-6) 7,8-Dimethoxy-3-(3-iodopropyl)- 1 ,3-dihydro-2H-3-benzazepin-2-one (Formula-4) (17.8g, 0.0456mol.) is added with (lS)-4,5-Dimethoxy-l-[(methylamino)methyl] benzocyclobutane hydrochloride (Formula-5) (9.29g, 0.0381mol.) in about 107ml. Acetone. To the mass, Potassium carbonate (12.7g, 0.0919mol.) is added and stirred for about 3hr. at 55 – 58C. The mass is filtered through celite bed at 35 – 40C. Filtrate is concentrated under reduced pressure at 45 – 50C to 1.4w/w. To the residual mass, 89ml of ethyl acetate is added and the product is extracted using 3N HC1 solution thrice (89ml, 2 x 35.6ml). The combined aqueous layer is basified using Sodium hydroxide and extracted the product using ethyl acetate thrice (89ml. 2 x 36.5ml). The combined organic layer is washed with water and then concentrated under vacuum at 45 – 50C to obtain about 19.29g (85%) of 3-{3-[(3,4-dimethoxy-bicyclo[4.2.0]octa-l,3,5-trien-7-ylmethyl)- methyl-amino]-propyl}-7,8-dimethoxy-l,3-dihydro-benzo[d]azepin-2-one (Formula-6) having the purity >75%>

The synthetic route of 148870-57-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BIOCON LIMITED; KOTHAKONDA, Kiran Kumar; RAMASAMY, Sivakumar; BANDARU, Sravan Kumar; VENKATA, Srinivas Pullela; WO2014/20534; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 13421-13-1, These common heterocyclic compound, 13421-13-1, name is 4-Chloro-2-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.

Example 3Amethyl 4-chloro-2-iodobenzoate To a solution of 4-chIoro-2-iodobenzoic acid (10.61 g, 37.62 mmol) in methanol (75 ml), trimethylsilyldiazomethane (30 ml, 2.0 M in ether) was added drop by drop. 1725 After 1 hour, another batch of trimethylsilyldiazomethane (26 ml, 2.0 M in ether) was added drop by drop. The reaction mixture was stirred at room temperature overnight and concentrated. The crude product was purified by column chromatography (0-20% ethyl acetate in hexanes) to yield the title compound.

The synthetic route of 13421-13-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBOTT LABORATORIES; ABBOTT LABORATORIES TRADING(SHANGHAI) COMPANY, LTD.; VAN CAMP, Jennifer; PATEL, Jyoti, R.; SWANN, Steven; WO2012/45194; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 5471-81-8, 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 5471-81-8 as follows.

A solution of methyl 4-iodo-3-methylbenzoate (21 .7 mmol, 6 g) in dry THF (120 mL) was purged with argon. The solution was cooled to -155C, /-PrMgCI (2M in THF, 108.5 mmol, 54.25 mL), and DMF (130.2 mmol, 10 mL) were added and the reaction was stirred for 2 h at -155C and then warmed to 255C and allowed to react for an additional hour. The reaction was quenched with aqueous 1 N HCI and extracted with EtAcO. The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated. The resulting crude was purified by flash chromatography on silica gel using an elution of 6% ethylacetate in hexanes to give methyl 4-formyl-3-methylbenzoate (3.08g .Yield: 80%). 1 H NMR (400 MHz, CDCI3) delta 10.35 (1 H, s), 8.00 (1 H, d, J=8Hz), 7.99 (1 H, s), 7.86 (1 H, d, J=8Hz), 3.95 (3H, s), 2.72 (3H, s) LC-MS: tR = 2.85 [M+H]+ = not ion (method 3).

According to the analysis of related databases, 5471-81-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ALMIRALL, S.A.; DRACONIS PHARMA, S.L.; LABORATORIOS DEL DR. ESTEVE, S.A.; AGUILAR, Nuria; FERNANDEZ, Joan, Carles; TERRICABRAS, Emma; CARCELLER GONZALEZ, Elena; SALAS SOLANA, Jordi; WO2013/149997; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 191348-14-8, A common heterocyclic compound, 191348-14-8, name is 2-Iodo-4-methoxyaniline, molecular formula is C7H8INO, 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.

Under anhydrous and anaerobic conditions, 0.1 mmol of 2-iodo-4-methoxyaniline was added.0.12 mmol of 3-bromo-4-methoxybenzaldehyde, 0.3 mmol of selenium powder,0.005 mmol of copper, 0.2 mmol of potassium hydroxide and 10 ml of DMSO solution,The reaction was refluxed at 120 C in a single-neck round bottom flask, and the reaction was monitored by TLC.Separation of pure methoxy-containing benzoselenazole compounds by column chromatographyThe reaction product was obtained by demethylation of boron tribromide (6 eq.). The product was obtained as pale yellow solid.The yield was 23%.

The synthetic route of 191348-14-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wuhan University; Zhou Haibing; Zhang Silong; Hu Zhiye; Li Yuanyuan; Ning Wentao; Dong Chune; (13 pag.)CN108863985; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 455-13-0, name is 4-Iodobenzotrifluoride, 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 4-Iodobenzotrifluoride

General procedure: A 25 mL Schlenk tube was charged with Cu2O (0.05 mmol), ArX (0.5 mmol), NHR1R2 (0.75 mmol), NaOH (1 mmol), TBAB (0.1 mmol), L2 (0.1 mmol) and H2O/EtOH (1 mL, 1/1, v/v). The mixture was stirred at 120 C for 12 h. The reaction mixture was extracted with ethyl acetate (3 10 mL), washed with water and brine, dried over anhydrous Na2SO4, and concentrated in vacuo. The residue was purified by flash column chromatograph on silica gel(ethyl acetate/petroleum ether as the eluent) to provide the target products 3a-3w and 6.

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

Reference:
Article; Xie, Jian-Wei; Yao, Zhen-Bin; Wang, Xiao-Chuang; Zhang, Jie; Tetrahedron; vol. 75; 27; (2019); p. 3788 – 3792;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com