Author: Jessica.F

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. 1219741-79-3, name is 4-Bromo-5-fluoro-2-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of 4-Bromo-5-fluoro-2-iodoaniline

To a mixture of 4-bromo-5-fluoro-2-iodoaniline (step 1) (5.2 g, 16 mmol), Pd(PPh3)2Cl2 (582 mg, 0.83 mmol) and CuI (313 mg, 1.6 mmol) in 50 ml of Et3N was added ethynyltrimethylsilane (2.3 mL, 1.6 mmol) slowly at 0 C. The resulting mixture was degassed and charged with N2 three times. After stirring at 30 C. for 2 hrs, the reaction mixture was filtered over celite. The filtrate was diluted with ethyl acetate (*2), washed with water (*2) and brine (*2). The combined organic layers were dried over anhydrous Na2SO4 and filtered. The filtration was evaporated under reduced pressure to afford the crude product, which was purified by column chromatography on silica gel eluting with 0?5% ethyl acetate in hexanes to afford the title compound as yellow oil. LC-MS: Rt=1.29 mins; MS m/z [M+H]+ 286.0; Method 5-95AB 1.5minLC_v003 1H NMR (400 MHz, CDCl3) delta 7.19 (1H, d), 6.21 (1H, d), 4.11 (2H, s), 0.00 (9H, s).

The synthetic route of 1219741-79-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; CHEN, Shuhui; HE, Haiyang; LAGU, Bharat; QIN, Hua; WU, Chengde; XIAO, Yisong; US2015/183802; (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. 188815-32-9, name is 3-Bromo-5-iodobenzoic acid, A new synthetic method of this compound is introduced below., SDS of cas: 188815-32-9

Example 50 Synthesis of 3-Bromo-5-hydroxy-benzoic acid; The title compound was made according to the method described in Org. Proc. Res. Dev. 2002, 6, 591-595. To 5- iodo-3-bromo-benzoic acid (500 mg, 1.53 mmol), NaOH (250 mg, 6.1 mmol), Cu20 (240 mg, 1.68 mmol) was added water (4.0 mL). The mixture was heated for 1.5 h at 140 C in a sealed tube. The cooled mixture was diluted with water and extracted with CH2Cl2. The aqueous layer was acidified (pH-2) with TFA and extracted with EtOAc. The organic layer was dried over Na2S04, filtered, concentrated and purified by reverse-phase HPLC to yield 3-bromo-5-hydroxy-benzoic acid. ?H NMR (400 MHz, DMSO-d6): 10.30 (s, 1H), 7.46 (m, 1H), 7.31 (m, 1H), 7.17 (m, 1H).

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; AMGEN INC.; WO2005/113494; (2005); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 610-97-9, A common heterocyclic compound, 610-97-9, name is Methyl 2-iodobenzoate, molecular formula is C8H7IO2, 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.

2.27 g (15 mmol) was added sequentially to a 250 mL round bottom flask.Methyl 2-aminobenzoate, 3.93 g (15 mmol) of methyl 2-iodobenzoate,2.49 g (18 mmol) of potassium carbonate, 0.19 g (3 mmol) of activated copper powder and100mL of o-dichlorobenzene, degassing the reaction system, and then protecting with argon gas,The mixture was heated to 180 C with stirring and the reaction was continued for 48 h. After the reaction is complete,The system was cooled to room temperature, suction filtered under reduced pressure and the residue was washed with dichloromethane.After the filtrate was spin-dried, it was separated and purified on a silica gel column using an eluent of dichloromethane: petroleum ether = 3:1 (volume ratio).Obtained a yellow-green solid 3.66g,The yield was 85.6%.

The synthetic route of 610-97-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Soochow University (Suzhou); Liao Liangsheng; Yuan Yi; Jiang Zuoquan; (46 pag.)CN109456326; (2019); A;,
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 1133123-02-0 as follows. Safety of 4-Bromo-2-iodobenzoic acid

General procedure: A sealed tube was charged with CuCl (0.02 mmol), BFMO (0.02 mmol), N-protected N-alkenylhydrazine (2.0 mmol), 2-iodobenzoic acid (2.4 mmol), and K2CO3 (4 mmol). The tube was evacuated and backfilled with argon three times before anhydrous DMSO (4.0 mL) was added via syringe (NOTE: for liquid substrates, they were added into the tube via syringe after the tube was backfilled with argon). The mixture was sealed and stirred at 80 C for 24 h. The mixture was diluted with EtOAc, washed with water, dried over anhydrous sodium sulfate, and filtrated. The filtrate was concentrated in vacuo and the residue was treated with 4M HCl/1,4-dioxane (1.2 mL) at 80 C. After the starting material was completely consumed, the solution was cooled and diluted with EtOAc. The resultant mixture was washed with water and dried over anhydrous sodium sulfate. After the solution was concentratedin vacuo, the residue was purified by flash chromatography to afford the corresponding indole.

According to the analysis of related databases, 1133123-02-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Wei, Quanpeng; Wang, Yunhan; Zhao, Jinlong; Zhang, Xiaojing; Ma, Dawei; Tetrahedron; vol. 76; 1; (2020);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 766-99-4, 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. 766-99-4, name is 1-Ethynyl-4-iodobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A 25 mL reaction flask was charged with ferrous chloride (0.05 mmol),4-iodophenylacetylene (0.5 mmol), 4-fluorobenzeneboronic acid (0.75 mmol),Sodium carbonate (1.0 mmol),Cesium hydroxide monohydrate (2.5 mmol),Sodium iodide (0.25 mmol),(0.75 mmol), & lt; / RTI & gt;Chloroform (1.5 mmol) and polyethylene glycol-400 (2.0 g),And reacted at 120 C for 6 h. Cooled to room temperature,extraction,The solvent was distilled off under reduced pressure, and the residue was isolated by column chromatography to give a yield of 87%.

The synthetic route of 1-Ethynyl-4-iodobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nanjing Normal University; HAN, WEI; DU, HONGYAN; (14 pag.)CN106116999; (2016); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

645-00-1, name is 1-Iodo-3-nitrobenzene, 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. Formula: C6H4INO2

EXAMPLE 3 6-(Furan-3-yl)-3-[3-(imidazol-1-yl)phenyl]-3 H -imidazo[4,5- b ]pyridine An intimate mixture of 1-iodo-3-nitrobenzene (24.9 g, 0.1 mol), copper bronze (320 mg, 5 mmol), potassium carbonate (15.2 g, 0.11 mol) and imidazole (15.0 g, 0.22 mol) was heated under a stream of nitrogen at 200C for 90 minutes. The reaction was cooled to 100C, carefully treated with water (750 ml) and the resulting suspension stirred to ambient temperature over 16 hours. Filtration gave a grey-coloured solid which was dissolved in hot toluene (125 ml) and treated with decolourising charcoal (2 g). Filtration and cooling afforded 1-(3-nitrophenyl)-1H-imidazole as pale green needles (13.5 g, 71%). deltaH (360 MHz, CDCl3) 7.29 (1H, br s), 7.38 (1H, br s), 7.68-7.78 (2H, m), 7.97 (1H, br s), 8.23-8.29 (2H, m).

The synthetic route of 645-00-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Merck Sharp & Dohme Limited; EP1214319; (2003); B1;,
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. 460-37-7, name is 1,1,1-Trifluoro-3-iodopropane, A new synthetic method of this compound is introduced below., Computed Properties of C3H4F3I

General procedure: 2-Thioadenosine (300 mg, 1 mmol) was dissolved with stirring in 7.5 ml DMF. Sodium dithionite (750 mg) was added and the mixture was stirred for 30 min under Ar. The reaction mixture was cooled in ice, aqueous sodium hydroxide (50% (w/w) solution (240 mg, 3 mmol) was added, and after 10 min stirring the alkyl iodide (1.1 mmol) was added dropwise over 10 min. The cooling was removed, and after 1 h stirring at rt the reaction mixture was analyzed by LCMS. If unreacted starting material was present an additional amount of alkyl iodide (0.134 mmol, 0.2 eqv.) was added with ice cooling, and after 1 h stirring at room temperature the analysis was repeated. When no starting material was present the reaction mixture was diluted with 75 ml of water and after ca. 2 h stirring the crude product was collected by filtration and washed with water. This material was purifiedby column chromatography on silica gel using chloroform/methanol as eluent.

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; Yanachkov, Ivan B.; Chang, Hung; Yanachkova, Milka I.; Dix, Edward J.; Berny-Lang, Michelle A.; Gremmel, Thomas; Michelson, Alan D.; Wright, George E.; Frelinger, Andrew L.; European Journal of Medicinal Chemistry; vol. 107; (2016); p. 204 – 218;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 612-55-5, These common heterocyclic compound, 612-55-5, name is 2-Iodonaphthalene, 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: A mixture of aryl halide (1.0 mmol), arylboronic acid (1.2 mmol), K2CO3 (2.0 mmol), DMF-H2O (3-3 ml), and n-dodecane (15-20 mg) as an internal GC standard and 0.5 mol% of catalyst was stirred at 80? C in air. Progress of the reaction was monitored by withdrawing the reaction mixtures periodically and analyzed by GC/GC-MS. GC yields were based on the amount of aryl halide employed. At the end of the reaction, the catalyst was separated by simple filtration. Filtrate was dried over Na2SO4, filtered, concentrated and the residue was purified by flash column chromatography on silica gel. The product was analyzed by GC-MS. All the prepared compounds are known and compared with authentic samples.

Statistics shows that 2-Iodonaphthalene is playing an increasingly important role. we look forward to future research findings about 612-55-5.

Reference:
Article; Islam, Sk. Manirul; Salam, Noor; Mondal, Paramita; Roy, Anupam Singha; Journal of Molecular Catalysis A: Chemical; vol. 366; (2013); p. 321 – 332;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Some common heterocyclic compound, 181765-86-6, name is Methyl 5-bromo-2-iodobenzoate, molecular formula is C8H6BrIO2, 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. name: Methyl 5-bromo-2-iodobenzoate

Step1: The reactor was added 9- phenanthrene boronic acid (2.22g, 10mmol),Methyl 5-bromo-2-iodobenzoate (3.41 g, 10 mmol), Pd(PPh3)4 (0.21 g, 0.18 mmol), K2CO3 solution (2.76 g, 20 mmol), 5 mL of deionized water,13 mL of toluene and 130 mL of tetrahydrofuran were stirred and refluxed for 12 hours. After the reaction was terminated,The organic layer was separated and distilled under reduced pressure.Through silica gel column purification, and dried to give intermediate 35-1 (2.86g, 73%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 181765-86-6, its application will become more common.

Reference:
Patent; Changchun Hai Purunsi Technology Co., Ltd.; Dong Xiuqin; Cai Hui; (23 pag.)CN109305943; (2019); A;,
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. 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 2-Iodo-1,3-dimethylbenzene

Add 0.2 mmol of potassium carbonate,0.005 mmol of tris (dibenzylideneacetone) dipalladium,1,3-bis (diphenylphosphine) propane 0.02mmol,18-crown-6-ether 0.1mmol,1,3-dimethyl-2-iodobenzene 0.1 mmol,1-fluoro-4- (pent-1-yn-1-yl) benzene 0.25 mmol and1 mL of N, N-dimethylformamide was added to a 15 mL reaction tube,Fill with nitrogen repeatedly 10 times, stir at room temperature for 15min, add 0.5mmol of water,Then placed in a reaction tray at 100 C for 16 hours; cooled to room temperature, the reaction solution was diluted with ethyl acetate, washed with water, the organic phase was dried over anhydrous Na2SO4, filtered, concentrated, and purified by thin-layer chromatography to obtain 14.1 mg of the target product. Color oil, 51% yield.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 608-28-6.

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (12 pag.)CN110256184; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com