Category: 13421-00-6

Electric Literature of 13421-00-6, 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 13421-00-6 as follows.

General procedure: A mixture of benzonitrile(2.0 mmol) and o-iodobenzoic acid (2.0 mmol) and [bmIm]OH (35mol) was stirred at room temperature for (3-5) h. After completion of reaction as indicated byTLC, 20mL of water was added to the reaction mixture and stirred well. The product was extracted with ether (3¡Á20 mL). The combined organic layers were dried over anhydrous Na2SO4 to afford the crude product, this crude product was taken to column in order to obtain analytically pure compound 4(a-m)(77-91%). After isolation of the product, the remaining aqueous layer containing the ionic liquid was washed with ether (2x10mL) to remove organic impurity and filtered. The filtrate was extracted with dichloromethane(2¡Á10mL), dried over MgSO4 and evaporated under reduced pressure to afford [bmIm]OH, which was reused five times in subsequent runs without further purification.

According to the analysis of related databases, 13421-00-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Waseem, Malik Abdul; Shireen; Srivastava, Anjali; Srivastava, Arjita; Rahila; Siddiqui; Tetrahedron Letters; vol. 55; 44; (2014); p. 6072 – 6076;,
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. 13421-00-6, name is 5-Chloro-2-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 5-Chloro-2-iodobenzoic acid

A solution of 5-chloro-2-iodobenzoic acid (3.0 g, 10.62 mmol), SOC12 (12 mL) and DMF (0.6 mL) was gently warmed with a heat gun until the mixture becamehomogeneous (15 mm). The solution was maintained at 23C for additional 30 mm and then the solution was concentrated. MeOH (24 mL) was added to the crude residue and the solution was maintained at 23C for 30 mm. The solution was concentrated and the residue was purified by flash chromatography on Biotage silica gel cartridge (cyclohexane to cyclohexane : EtOAc = 85 : 15) to afford methyl 5-chloro-2-iodobenzoate (3.02 g, 10.20 mmol, 96%).UPLC-MS: 1.17 mm, 296.6 [M+H]+, method 12.

The synthetic route of 13421-00-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CHIESI FARMACEUTICI S.P.A.; BIAGETTI, Matteo; CAPELLI, Anna Maria; ACCETTA, Alessandro; CARZANIGA, Laura; WO2015/91685; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 13421-00-6, A common heterocyclic compound, 13421-00-6, name is 5-Chloro-2-iodobenzoic acid, molecular formula is C7H4ClIO2, 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.

Reference Example 2-66 5-Chloro-2-[[1-(2-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid Following the procedure described in Reference Example 2-5, the title compound was prepared from 5-chloro-2-iodobenzoic acid and 1-(2-pyridinyl)-1H-pyrazol-5-ylamine (88% yield). mp: 233-234 C. (recrystallized from ethanol). NMR (DMSO-d6) delta: 6.42 (1H, d, J=2.0 Hz), 7.38 (1H, ddd, J=1.2 Hz, 4.8 Hz, 7.4 Hz), 7.54 (1H, dd, J=2.6 Hz, 8.8 Hz), 7.63 (1H, d, J=8.8 Hz), 7.71 (1H, d, J=2.0 Hz), 7.88-7.92 (2H, m), 7.99-8.08 (1H, m), 8.47 (1H, dd, J=0.8 Hz, 1.8 Hz, 4.8 Hz), 12.24 (1H, br s), hidden (1H).

The synthetic route of 13421-00-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Uchikawa, Osamu; Mitsui, Keita; Asakawa, Akiko; Morimoto, Shigeru; Yamamoto, Masataka; Kimura, Hiroyuki; Moriya, Takeo; Mizuno, Masahiro; US2003/187014; (2003); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 13421-00-6, A common heterocyclic compound, 13421-00-6, name is 5-Chloro-2-iodobenzoic acid, molecular formula is C7H4ClIO2, 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.

According to the procedure reported by Yu and co-workers [3], palladium acetate (22 mg, 0.10mmol), iodobenzene diacetate (644 mg, 2.0 mmol), iodine (507 mg, 2.0 mmol), and tetrabutylammonium iodine (739 mmol, 2.0 mmol) were added to a solution of 3-chlorobenzoic acid (313 mg, 2.0 mmol) in 1,2-dichloroethane (20 mL). The mixture was heated at 100 C with stirring for 2 h and then allowed to cool to room temperature. Iodobenzene diacetate (644 mg, 2.0 mmol) and iodine (507 mg, 2.0 mmol) were added to the mixture. After stirring at 100 C for 4 h, the resulting mixture was diluted with10% sodium carbonate. The aqueous layer was separated, washed with Et2O, and then acidified with 10% HCl. The resulting mixture was extracted with EtOAc and the organic layer was dried over Na2SO4; filtered; and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/EtOAc = 4/1) to give crude 5-chloro-2-iodobenzoic acid (223 mg) as a colorless solid, which was suspended in thionyl chloride (2 mL). After stirring under reflux conditions for 2 h, the resulting mixture was concentrated under reduced pressure. The remaining thionyl chloride was removed by azeotropic distillation with benzene. The residue was dissolved in anhydrous CH2Cl2 (3 mL). To the mixture were added isopropylamine (56 mg, 0.95 mmol) and triethylamine (240 mg,2.37 mmol) at 0 C under a nitrogen atmosphere. After stirring at room temperature for 13 h, the resulting solution was diluted with EtOAc. The mixture was washed with 10% HCl, saturated aqueous NaHCO3, water, and brine; dried overNa2SO4; filtered; and concentrated under reduced pressure. The residue was purified by recrystallization from hexaneand CHCl3 to give 19 (138 mg, 21% in 3 steps) as colorless needles.

The synthetic route of 13421-00-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yakura, Takayuki; Fujiwara, Tomoya; Yamada, Akihiro; Nambu, Hisanori; Beilstein Journal of Organic Chemistry; vol. 14; (2018); p. 971 – 978;,
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. 13421-00-6, name is 5-Chloro-2-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 5-Chloro-2-iodobenzoic acid

General procedure: A dry sealable vial was charged with sulfonimidamide 4a (368 mg, 2.00 mmol), 2-iodobenzoic acid (494 mg, 2.00 mmol), CuI (76 mg, 0.40 mmol), and K2CO3 (690 mg, 5.00 mmol) in anhyd DMF (5.0 mL). After heating to 100 C for 2 h, the heterogeneous mixture was cooled to r.t. The mixture was diluted with water (10 mL), acidified with 2 M HCl and extracted with EtOAc (3 ¡Á 30 mL). The combined organic layers were dried (Na2SO4), filtered, and concentrated under reduced pressure. The crude product was purified by CombiFlash chromatography (silica gel, n-hexane/EtOAc, 6:4) to afford the desired product 7a as a cream solid; yield: 633 mg (90%).

The synthetic route of 13421-00-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sen, Indira; Sasmal, Swarnendu; Hall, Roger G.; Pal, Sitaram; Synthesis; vol. 48; 21; (2016); p. 3743 – 3752;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 13421-00-6,Some common heterocyclic compound, 13421-00-6, name is 5-Chloro-2-iodobenzoic acid, molecular formula is C7H4ClIO2, 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.

Borane-dimethylsulfide complex (3.7 mL, 38.9 mmol) was added slowly to a cold (0C) solution of 5-chloro-2-iodo-benzoic acid (10 g, 35.4 mmol) in THF (20 mL). The reaction mixture was allowed to warm to rt, stirred for 8 h, quenched by addition of a saturated aqueous solution of ammonium chloride, and extracted with EtOAc. The organic layer was dried (Na2S04), filtered, and concentrated to provide 9.5 g of the title compound. tR: 4.72 min (HPLC 2); Rf= 0.66 (hexane/EtOAc, 7:3).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Chloro-2-iodobenzoic acid, its application will become more common.

Reference:
Patent; NOVARTIS AG; FURET, Pascal; GUAGNANO, Vito; HOLZER, Philipp; MAH, Robert; MASUYA, Keiichi; SCHLAPBACH, Achim; STUTZ, Stefan; VAUPEL, Andrea; WO2013/80141; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

13421-00-6, name is 5-Chloro-2-iodobenzoic acid, 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. 13421-00-6

To a solution of 5-chloro-2-iodobenzoic acid (3.0 g, 10.6 mmol) in toluene (150 mL), SOCl2 (7.75 mL, 106 mmol) was added and the mixture was heated at 100 C. for 3 hours. The solvent was concentrated in vacuum and the residue was co-evaporated from toluene twice to give the title compound as a grey solid. Yield (3.2 g, 100%) [0177] 1H NMR (400 MHz, CDCl3): delta 7.26 (dd, 1H), 7.98 (d, 1H), 8.03 (d, 1H).

Statistics shows that 13421-00-6 is playing an increasingly important role. we look forward to future research findings about 5-Chloro-2-iodobenzoic acid.

Reference:
Patent; Stasi, Luigi Piero; Rovati, Lucio Claudio; US2015/65523; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com