Month: February 2021

Electric Literature of 25252-00-0,Some common heterocyclic compound, 25252-00-0, name is 2-Bromo-5-iodobenzoic acid, molecular formula is C7H4BrIO2, 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.

Oxalyl chloride (13.0 mL) is added to an ice-cold solution of 2-bromo-5-iodo-benzoic acid (49.5 g) in CH2CI2 (200 mL). DMF (0.2 mL) is added and the solution is stirred at room temperature for 6 h. Then, the solution is concentrated under reduced pressure and the residue is dissolved in THF (100 mL). The resulting solution is cooled in an ice-bath and L1BH4 (3.4 g) is added in portions. The cooling bath is removed and the mixture is stirred at room temperature for 1 h. The reaction mixture is diluted with THF and treated with 0.1 M hydrochloric acid. Then, the organic layer is separated and the aqueous layer is extracted with ethyl acetate. The combined organic layers are dried (Na2S04) and the solvent is evaporated under reduced pressure to give the crude product. Yield: 47.0 g (99% of theory)

The synthetic route of 25252-00-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM VETMEDICA GMBH; KLEY, Saskia; REICHE, Dania Birte; WO2015/110402; (2015); 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. 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, A new synthetic method of this compound is introduced below., SDS of cas: 103962-05-6

A solution of 3-(4-bromophenyl)-lH-l,2,4-triazole (10.9 g, 48.5 mmol), l-iodo-4-(trifluoromethoxy)benzene (13.2 g, 45.8 mmol), copper(I) iodide (2.38 g, 12.5 mmol), and cesium carbonate (30.3 g, 93.0 mmol) in dimethylsulfoxide (85 mL) was degassed with nitrogen for 5 minutes. The mixture was heated at 100 ¡ãC for 60 hours. After cooling, ethyl acetate (200 mL) was added and the mixture was filtered through Celite?. The filtrate was added to a solution of saturated ammonium chloride (200 mL) and stirred for one and a half hours. The layers were separated and the aqueous layer was extracted with ethyl acetate (3 x 100 mL). The combined organic extracts were dried over anhydrous magnesium sulfate, filtered, and adsorbed onto Celite?. Purification by flash column chromatography using 0-40percent ethyl acetate/hexanes as eluent provided the title molecule as an off-white solid (9.65 g, 52percent) : mp 109-112 ¡ãC; XH NMR (400 MHz, CDCI3) delta 8.56 (s, 1H), 8.10-8.03 (m, 2H), 7.83-7.75 (m, 2H), 7.64-7.57 (m, 2H), 7.42-7.35 (m, 2H); ESIMS m/z 384 ([M + H]+).

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; DOW AGROSCIENCES LLC; GIAMPIETRO, Natalie C.; BAUM, Erich W.; FISCHER, Lindsey G.; GOLDSMITH, Miriam E.; CROUSE, Gary D.; RENGA, James M.; SPARKS, Thomas C.; (234 pag.)WO2016/99929; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 116632-39-4, name is 5-Bromo-2-iodotoluene, 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: 5-Bromo-2-iodotoluene

[0001074] To a mixture of Compound 298A (2.96 g, 0.01 mol), 4-fluorophenylboronic acid (2 g, 1.32 mol), and K3PO4 (6.4 g, 0.03 mol) in 1 ,2-dimethoxyethane (80 mL) was added Pd(dppf)Cl2 (733 mg, 1.0 mmol). The reaction mixture was stirred under nitrogen at room temperature overnight. The resulting mixture washed with brine (100 mL), dried over anhydrous sodium sulfate, filtered, and concentrated. The residue was purified with flash column chromatography on silica gel (ethyl acetate in petroleum ether, from 10% to 50% v/v) to furnish Compound 298B.

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

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; CHU, Daniel; BRIDGES, Alexander, James; WO2015/42397; (2015); A1;,
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. 624-75-9, name is 2-Iodoacetonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Computed Properties of C2H2IN

General procedure: Starting amine (5.0 mmol) was dissolved in dry diethyl ether (17 mL) and iodoacetonitrile (5.5 mmol, 919 mg) was added dropwise under cooling. The mixture was stirred at room temperature for 3-14 days, then precipitate was filtered off, washed with diethyl ether and dried in vacuo to give the corresponding quaternary ammonium salt 2. If the solid precipitate was not formed after 7 days, the mixture was evaporated under reduced pressure. The crude product was washed with diethyl ether (3 ¡Á 15mL) and dried in vacuo. The quaternary ammonium salt 2 was used in the next step without additional purification. The corresponding quaternary ammonium salt (3.0 mmol) was heated at 150 C on oil bath in freshly distilled DMF (7 mL) in a 25 mL round-bottom flask fitted with reflux condenser and CaCl2-tube for 15 minutes. The mixture was cooled to room temperature, diluted with H2O (20 mL) and extracted with PhMe (2 ¡Á 15mL). The organic phase then was washed with H2O (2 ¡Á 15mL) and brine (15 mL), dried over Na2SO4 and evaporated in vacuo to give the desired aminoacetonitrile 4. The latter, if necessary, was purified by column chromatography (it is convenient to visualize aminoacetonitriles on TLC-plate by treating with the diluted solution of ninhydrin in EtOH). Note, that aminoacetonitriles are moisture sensitive. Products after column chromatography were additionally dried by the addition of dry PhMe (5 mL) and evaporation in vacuo.

The synthetic route of 624-75-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Buev, Evgeny M.; Smorodina, Anastasia A.; Stepanov, Maxim A.; Moshkin, Vladimir S.; Sosnovskikh, Vyacheslav Y.; Tetrahedron Letters; vol. 59; 17; (2018); p. 1638 – 1641;,
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. 217314-45-9, name is Methyl 3-amino-5-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 217314-45-9

Step C: To a 0C solution of aniline from step B (21.7 g, 78.3 mmol) in 3:1 DCM:pyridine (75 mL) wasadded methanesulfonyl chloride (6.36 mL, 82.2 mmol). The ice bath was removed after 15 min and thesolution was stirred overnight at rt. The reaction mixture was extracted several times with IN HC1. Theorganic phase was dried, concentrated, and cliromatographed (1:1 EtOAc:Hex) to afford the desiredsulfonamide as a white solid.

The synthetic route of 217314-45-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK & CO., INC.; WO2006/2004; (2006); 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. 6828-35-9, name is 5-Chloro-2-iodoaniline, A new synthetic method of this compound is introduced below., Application In Synthesis of 5-Chloro-2-iodoaniline

1 mmol of 5-chloro-2-iodoaniline was added to the reaction vessel, 3 mL of aqueous ammonia at 12 mol / L and 1 mmol of benzaldehyde were added 0.1 mmol of copper chloride, 0.1 mmol of proline lithium (proline lithiumas) Sodium hydroxide 3 mmol, water 3 mL. Placed in a microwave reactor at 150 w of power heated to 100 C for 15 min continuous reaction. After completion of the reaction, the mixture was cooled to room temperature and concentrated under reduced pressure. The product was purified by column chromatography to give a white solid in 86% yield.

The synthetic route of 6828-35-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Fujian Medical University; Ke Fang; Zhang Peng; Xu Jianhua; Wu Wen; Zheng Yu; Wu Lixian; (9 pag.)CN106866543; (2017); A;,
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. 51411-81-5, name is 3-Amino-4-iodobenzoic acid, A new synthetic method of this compound is introduced below., Application In Synthesis of 3-Amino-4-iodobenzoic acid

Step 3 Reaction with 1-Hexyne and Trifluoroacetylation To a mixture of 3-amino-4-iodobenzoic acid on Wang resin (loading 0.6 mmol/g; 3.0 g, 1.8 mmol) and 1-hexyne (0.74 g, 9.0 mmol) in DMF (40 mL) was added bis(triphenylphosphine)palladium(II) chloride (0.20 g, 0.28 mmol) and CuI (0.1 g, 0.52 mmol). The mixture was stirred magnetically for 2 h, filtered, and washed with CH2 Cl2. The resin was suspended in CH2 Cl2 (40 mL), cooled (0 C.), and pyridine (1.5 mL) and trifluoroacetic anhydride (2.6 mL) were added. After 2 h, the mixture was filtered, washed with CH2 Cl2, and dried. To confirm that the reactions occured, 100 mg of resin was treated with 50% TFA/CH2 Cl2 for 3 h, filtered, and the filtrate was concentrated to give 9.8 mg of 4-(1-hexynyl)-3-trifluoroacetamidobenzoic acid; 1 H NMR (DMSO-d6) delta 0.95 (t, 3 H), 1.50 (m, 4 H), 2.95 (m, 2 H), 7.60 (d, 1 H), 7.85 (d, 1 H), 7.90 (s, 1 H), 11.20 (s, 1 H). Anal. calc’d for C15 H14 F3 NO3: C, 57.51; H, 4.50; N, 4.47; Found: C, 57.20; H, 4.38; N, 4.46.

The synthetic route of 51411-81-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; American Home Products Corporation; US5932743; (1999); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 148836-41-3,Some common heterocyclic compound, 148836-41-3, name is 1-Bromo-4-chloro-2-iodobenzene, molecular formula is C6H3BrClI, 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: An oven-dried Schlenk tube was charged with a magneticstir bar, binucleophile 2-mercaptobenzimidazole 2 (1.0 mmol, 1.0 equiv), CuI(0.1 mmol, 10 mol %), phen (0.2 mmol, 20 mol %), and K2CO3 (2.0 mmol, 2equiv). The tube was capped and then evacuated and backfilled with nitrogen(3 times). Under a positive pressure of nitrogen, a solution of o-dihaloarene 1(1.05 mmol, 1.05 equiv) in DMF (3 mL) was added via syringe. The tube wassealed and allowed to stir at 120 C (monitored by TLC). After being cooled toroom temperature, EtOAc (40 mL) was added and the mixture was washedwith brine (20 mL 3). The organic phase was dried over Na2SO4 andconcentrated. The residue was purified by column chromatography on silicagel using petrol/EtOAc (10:1?3:1, v:v) as eluent to give product 3.

The synthetic route of 148836-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gao, Jilong; Zhu, Jiaoyan; Chen, Lubin; Shao, Yingying; Zhu, Jiaqi; Huang, Yijia; Wang, Xiaoxia; Lv, Xin; Tetrahedron Letters; vol. 55; 22; (2014); p. 3367 – 3373;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 6937-34-4, These common heterocyclic compound, 6937-34-4, name is 3-Iodophthalic 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.

[0591] To a solution of 3-iodophthalic acid (5.0 g, 17.1 mmol) in THF (75 mL) was added acetic anhydride (25 mL) at rt. The mixture was heated to 85C and stirred for 6 hrs. The reaction was cooled to rt and concentrated, providing 4-iodoisobenzofuran-1,3- dione (4.59 g, 98% yield) as a yellow solid. MS (ESI) m/z = 275 [M+H]+. 1H NMR (DMSO-d6, 400 MHz) ^: 8.39 (d, J = 8.0 Hz, 1 H), 8.06 (d, J = 7.2 Hz, 1 H), 7.66 (t, J = 7.6 Hz, 1 H).

Statistics shows that 3-Iodophthalic acid is playing an increasingly important role. we look forward to future research findings about 6937-34-4.

Reference:
Patent; BIOTHERYX, INC.; CHAN, Kyle, W.H.; FUNG, Leah; SULLIVAN, Robert; ERDMAN, Paul, E.; MERCURIO, Frank; (225 pag.)WO2017/201069; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 181765-85-5, 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. 181765-85-5, name is Methyl 4-chloro-2-iodobenzoate belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Methyl 4-chloro-2-iodobenzoate (284 mg, 0.96 mmol) is dissolved in DMF (2 mL) then methyl 2-acetamidoacrylate (205 mg, 1 .44 mmol), tetrabutylammonium bromide (308 mg, 0.96 mmol), NaHCO3 (201 mg, 2.39 mmol) and palladium (II) acetate (1 1 mg, 0.05 mmol) are added. The reaction mixture is heated at 85-90 C for 20 h under argon atmosphere. At the begining the reaction mixture is red, but after 10 min turned to dark red. After 20 h the reaction mixture is cooled to rt and 25 mL of water are added. The heterogenous solution is filtered, washed with small portions of water and dried to give the title compound (157 mg, 69%) as a brown solid. 1H-NMR (200 MHz, DMSO-de), delta: 3.86 (s, 3H); 7.41 (s, 1 H); 7.64 (d, 8.8 Hz, 1 H); 8.05 (s, 1 H); 8.20 (d, 8.8 Hz, 1 H). LC-MS: 238 [M+H].

The synthetic route of Methyl 4-chloro-2-iodobenzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERZ PHARMA GMBH & CO. KGAA; ABEL, Ulrich; HANSEN, Angela; WOLTER, Falko Ernst; KRUEGER, Bjoern; KAUSS, Valerjans; ROZHKOVS, Jevgenijs; PISKUNOVA, Irena; ZVAGULIS, Artis; TRIFANOVA, Dina; GRUNSTEINE, Ginta; TURE, Anastasija; WO2013/30358; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com