Tag: M.W=200-300

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. 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 3032-81-3

General procedure: A Schlenk tube with a magnetic stir bar was charged with Pd(OAc)2 (10 molpercent, 0.0056 g), AgOTf (1.1 equiv., 0.0707 g), TBAB (20 molpercent, 0.0161g), 2-phenylpyridine N-oxides 1 (0.25 mmol), iodobenzene and its derivatives 2 (0.375 mmol) and H2O (1 mL). The resulting solution was stirred at 100¡ãC for 12 h. The resulting organic layer was extracted with trichloromethane, treated with Na2SO4 and concentrated in vacuo. The product was isolated by short column chromatography using ethyl acetate and methanol as eluent.

According to the analysis of related databases, 3032-81-3, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhang, Wei; Li, Zhengkai; Zhang, Yihan; Yang, Li; Zhou, Xiangge; Synthetic Communications; vol. 47; 8; (2017); p. 793 – 802;,
Iodide – Wikipedia,
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Reference of 335349-57-0,Some common heterocyclic compound, 335349-57-0, name is 5-Chloro-4-iodo-2-nitroaniline, molecular formula is C6H4ClIN2O2, 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 E6 5-(2-tert.-Butoxy-ethoxy)-4-iodo-2-nitro-phenylamine Prepared from 5-chloro-4-iodo-2-nitro-phenylamine (Example A1) (14.9 g, 50 mmol), 2-tert.-butoxyethanol (29.5 g, 250 mmol) and KOH (3.99 g, 60 mmol) in DMSO (25 mL) at 23 C. according to the general procedure E. Obtained as a yellow solid (14.3 g). MS (ISP) 381 [(M+H)+]; mp 144-146 C.

The synthetic route of 335349-57-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoffmann-la Roche Inc.; US6407094; (2002); B1;,
Iodide – Wikipedia,
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Application of 13421-13-1, A common heterocyclic compound, 13421-13-1, name is 4-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.

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,
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Application of 2996-30-7, 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. 2996-30-7, name is 3-Fluoro-4-iodonitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 7A N-(2-Fluoro-4-nitrophenyl)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridine-4-amine 50 mg (0.19 mmol) of 1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridine-4-amine, 61 mg (0.23 mmol) of 2-fluoro-1-iodo-4-nitrobenzene and 26 mg (0.27 mmol) of sodium tert-butoxide are initially charged in 1 ml of toluene. The mixture is degassed. 8.7 mg (0.01 mmol) of tris(dibenzylideneacetone)dipalladium and 9.1 mg (0.02 mmol of dicyclohexyl(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine are then added. The mixture is heated in a sealed vessel at 120 C. overnight. The mixture is then filtered through an Extrelut cartridge (mobile phase: dichloromethane/methanol 10:1) and purified by preparative HPLC. Yield: 38 mg (50% of theory) LC-MS (Method 3): Rt=2.73 min. MS (ESI pos.): m/z=403 [M+H]+. 1H-NMR (DMSO-d6, 300 MHz): delta=-0.09 (s, 9H), 0.82 (t, 2H), 3.52 (t, 2H), 5.60 (s, 2H), 6.50 (d, 1H), 6.84 (d, 1H), 7.37 (t, 1H), 7.50 (d, 1H), 8.04 (dd, 1H), 8.13 (d, 1H), 8.17 (dd, 1H), 9.33 (s, 1H).

The synthetic route of 3-Fluoro-4-iodonitrobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bayer HealthCare AG; US2008/269268; (2008); A1;,
Iodide – Wikipedia,
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Synthetic Route of 124700-41-0, 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. 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Intermediate 11Z)-Ethyl 3-(dimethylamino)-2-(2-fluoro-5-iodobenzoyl)acrylate2-Fluoro-5-iodobenzoic acid (5.20 g, 19.55 mmol, Aldrich) was suspended in thionyl chloride (1.427 mL, 19.55 mmol, Aldrich) and heated to reflux for 30 min. The reaction mixture was cooled to room temperature and concentrated under reduced pressure to a tan solid. The solid was dissolved in toluene (30 mL) and concentrated under reduced pressure again. To a solution of the resulting solid (5.20 g, 19.55 mmol) in toluene (30 mL) was added triethylamine (2.72 mL, 19.55 mmol, Acros) and (Z)-ethyl 3-(dimethylamino)acrylate (3.64 mL, 25.41 mmol, Acros) and the reaction mixture was heated to 90 C. for 1 h. The reaction mixture was diluted with water and extracted three times with ethyl acetate. The combined organic extracts were dried over magnesium sulfate, filtered and concentrated under reduced pressure. Purification by Isco column (0%-100% ethyl acetate/dichloromethane) afforded the desired compound as a yellow solid (6.51 g).MS (ES) (M+H)+: 392 for C14H15FINO3 1H NMR: 0.88 (t, 3H), 2.78 (s, 3H), 3.33 (s, 3H), 3.85 (q, 2H), 7.03 (dd, 1H), 7.65 (dd, 1H), 7.77 (s, 2H).

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

Reference:
Patent; ASTRAZENECA AB; US2010/317624; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid, molecular formula is C7H4FIO2, 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. Application In Synthesis of 2-Fluoro-5-iodobenzoic acid

A stirred suspension of 2-fluoro-5-iodobenzoic acid (99.7 g) in DCM (1 L) at 200C was treated with oxalyl chloride (49.8 mL) and DMF (0.3 mL). After 3 h further DMF (0.1 mL) was added. After a further 2 h the clear solution was evaporated and re-evaporated from toluene (3 x 200 mL). The acid chloride was re-dissolved in toluene (1.5 L) and treated with triethylamine (79.2 mL) and ethyl 3-(dimethylamino)acrylate (65.3 g). After stirring for 2.5 h at 900C the mixture was filtered and evaporated. The residue was redissolved in EtOAc, washed with saturated sodium hydrogen carbonate solution (2x), water, saturated brine, dried (MgSO4) and treated with decolourising charcoal for 0.5 h. The mixture was filtered, evaporated, redissolved in diethyl ether and allowed to crystallise. The solid was filtered off, washed with diethyl ether and dried to give the title compound (91.2 g). On concentration and seeding a second crop was obtained (9.0 g); ESMS m/z 391.9 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 124700-41-0, its application will become more common.

Reference:
Patent; GLAXO GROUP LIMITED; WO2007/54295; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 181765-85-5, A common heterocyclic compound, 181765-85-5, name is Methyl 4-chloro-2-iodobenzoate, molecular formula is C8H6ClIO2, 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.

Preparation 20 Methyl 2-((tran-s,-2-((tert-butoxycarbonyl)amino)cyclopentyl)ethynyl)-4-chlorobenzoate Add diisopropylamine (0.44 mL, 3.11 mmol) to a solution of (¡À)-tert-butyl N-(trans- 2-ethynylcyclopentyl)carbamate (0.65 g, 3.11 mmol) and methyl 4-chloro-2-iodobenzoate (1.11 g, 3.73 mmol) in tetrahydrofuran (12 mL). Purge the solution with nitrogen for 5 minutes. Add copper(I) iodide (11.8 mg, 0.062 mmol) and bis(triphenylphosphine) palladium(II) chloride (43 mg, 0.062 mmol). Stir the mixture at room temperature overnight. Quench the reaction with water (50 mL) and extract with EtOAc (3 x 50 mL). Combine the organic extracts; wash with brine (50 mL); collect the organic layer; dry over MgS04; filter; collect the filtrate; and concentrate under reduced pressure. Subject the resulting crude material to silica gel flash chromatography, eluting with a gradient of 0% to 50% EtOAc in hexanes, to provide the title compound as a light yellow solid (0.57 g, 49%). ESMS (m/z) (35C1/37C1) 400/402 (M+Na)+.

The synthetic route of 181765-85-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; FISHER, Matthew Joseph; KUKLISH, Steven Lee; PARTRIDGE, Katherine Marie; YORK, Jeremy Schulenburg; (79 pag.)WO2016/69374; (2016); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

608-28-6, name is 2-Iodo-1,3-dimethylbenzene, 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. name: 2-Iodo-1,3-dimethylbenzene

General procedure: A 10 mL 2 dram screwed tube equipped with a magnetic stirring bar was charged with 5-vinyl-1,2,4-triazole (0.17 mmol, 1.0 equiv), an organic halide (0.17 mmol, 1.0 equiv), and K3PO4 (108 mg, 0.32 mmol, 2.0 equiv); then Pd(OAc)2 (1.7 mg, 0.008 mmol) were added, followed by DMF (1.0 mL), which was added to the mixture via syringe at r.t. under argon. The tube was sealed and put into a preheated oil bath at 110 C for 4 h. The mixture was cooled to r.t quenched with H2O (20 mL). The layers were separated and the aqueous layer was extracted with Diethyl Ether (3 ¡Á 20 mL). The combined organic extracts were dried (MgSO4), filtered, and concentrated in vacuo. The crude product was then purified by preparatory TlC [silica gel, EtOAc-PE, 3-7].

The synthetic route of 608-28-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Azzouni, Safa; Gaucher, Anne; Prim, Damien; Efrit, Mohamed Lotfi; Tetrahedron; vol. 76; 8; (2020);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 103962-05-6, 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. 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

At room temperature, 2-nitro-4-methoxybenzoic acid (0.4 mmol, 1 equiv), elemental selenium (1.2mmol, 3equiv), 4- trifluoromethoxy-iodobenzene (1.2mmol, 3equiv), Cu (OAc) 2 (0.04mmol), 1,10- phenanthroline (0.04 mmol), potassium carbonate (1.2mmol, 3equiv) and 2mL of toluene was added to the reaction tube, then filled with oxygen, and substituted three times, the oxygen the reaction environment, the reaction was stirred at a temperature of 100 deg.] C 24h. By the end of the reaction was monitored by thin layer chromatography, the reaction mixture was cooled, filtered and then ethyl acetate was added, and then spin off the solvent, the product obtained was isolated by column chromatography (eluent: petroleum ether: diethyl ether = 98), the product is yellow liquid, yield 91percent, by weight of the product is 143mg.

The synthetic route of 1-Iodo-4-(trifluoromethoxy)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wenzhou Medical University; Wu Ge; (20 pag.)CN107188841; (2017); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 111771-08-5, A common heterocyclic compound, 111771-08-5, name is 2-Fluoro-6-iodobenzoic acid, molecular formula is C7H4FIO2, 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: Preparation of Intermediates 4 To a mixture of 2-iodine benzoic acids 1 (4 mmol), 1-ethyl-3-(3-dimethyllaminopropyl)carbodiimide hydrochloride (4.8 mmol)and N-hydroxybenzotrizole (0.48 mmol) were added amines(4.8 mmol) at room temperature. The reaction mixture wasstirred overnight and washed with water successively. Theorganic layer was dried over anhydrous sodium sulfate. Then,the solvent was removed under vacuum to afford crude com-pounds 2. 2-Iodine benzamides 2 (3.00 mmol) were added to30 mL triethylamine in a round-bottom flask, then the solutionwas degassed with nitrogen for 10 min. CuI (0.306 mmol) andPdCl2(PPh3)2 (0.1044 mmol) were added and the system wasplaced under nitrogen atmosphere. Trimethylsilylacetylene(6 mmol) was added dropwise over 3 min. And the mixture washeated with stirring at 608C overnight. The reaction was allowedto cool to room temperature and then filtered over Celite. Thefiltrate was concentrated and purified by column chromatogra-phy on silica gel with petroleum ether and ethyl acetate as sol-vents to give the intermediates 3. Then, compounds 3(1.73 mmol) were added to 15mL MeOH in a flask and mixedwith K2CO3 (1.73 mmol). The flask was placed under nitrogenatmosphere and the system was stirred for 15 min, after whichH2O was added to the flask. The organic layer was extractedwith ethyl acetate, dried over Na2SO4, and concentrated undervacuum. The crude oil was then purified by column chroma-tography on silica gel to get structures 4.

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:
Article; Li, Jiling; Zhang, Zhicheng; Xu, Xiaoyong; Shao, Xusheng; Li, Zhong; Australian Journal of Chemistry; vol. 68; 10; (2015); p. 1543 – 1549;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com