Tag: M.W=200-300

Synthetic Route of 2974-94-9, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2974-94-9 name is 1-Iodo-4-phenoxybenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Compound 4: 25 mL reaction flask was charged with 4-phenoxyiodobenzene (0.5 mmol), 3-ethoxyphenylboronic acid (0.75 mmol), sodium carbonate (1.0 mmol), and cesium hydroxide monohydrate (2.5 mmol), sodium iodide (0.25 mmol), pivalic acid (0.75 mmol), chloroform (1.5 mmol) and ethylene glycol (2.0 g). Reacted at 120 C for 24 h. Cool to room temperature, extract, the solvent was evaporated under reduced pressure and then purified by column chromatography to yield a yield of 92%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Iodo-4-phenoxybenzene, and friends who are interested can also refer to it.

Reference:
Patent; Nanjing Normal University; Han Wei; Xu Fangning; (15 pag.)CN108774122; (2018); 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. 90347-66-3, name is Methyl 3-iodo-4-methylbenzoate, A new synthetic method of this compound is introduced below., SDS of cas: 90347-66-3

A mixture of 4 (7.26 g, 26.3 mmol), 11(3.0 g, 17.5 mmol), K2C03 (4.84 g, 35.0 mmol), DMEDA (386 mg, 4.38 mmol) and Cul (834 mg, 0.871 mmol) in 90 ml of dioxanewas stirred at 100 C under N2 for 18h. The mixture was filtered, concentrated and purified by column chromatography to give 12 (2.2 g, 39%) as a slightly yellow solid. LCMS (m/z: m+1): 320.2.

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; CARDIO THERAPEUTICS PTY LTD; TREUTLEIN, Herbert; ZENG, Jun; DIXON, Ian; JAMES, Ian; PALMER, James T; (169 pag.)WO2018/165718; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Electric Literature of 160938-18-1, 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. 160938-18-1, name is 4-Chloro-2-iodo-1-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows.

The obtained from step-1 5- (4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl) -1H-indole 22 g (90.5 mmol) and 4-chloro-2-iodo -1-nitrobenzene 28.2 g of purified water was added to 250 mL and dioxane 500 mL (100 mmol).Pd (PPh3) 45.2 g (4.5 mmol), K2CO338 g (271 mmol) was added and the mixture was heated under reflux for 12 hours at 120 .Allowed to cool to room temperature and quench the reaction with 500 mL aqueous solution of ammonium chloride to the reaction mixture.Extract the mixture with EA 500 mL, and washed with distilled water.The resulting organic layer was dried over anhydrous MgSO4,and evaporated under reduced pressure to obtain the desired compound 19.7 g (80% yield) was purified by silica gel column chromatography.

The chemical industry reduces the impact on the environment during synthesis 4-Chloro-2-iodo-1-nitrobenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; DoosanCorporation; Sim, Jae Uii; Lee, In Hyuk; Baek, Young Mi; Sin, Jin Yong; Park, Ho Chul; Lee, Chang Jun; Lee, Uhn Jung; Kim, Tae Hyung; Lee, Jae Hun; (35 pag.)KR101571592; (2015); 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. 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, A new synthetic method of this compound is introduced below., name: 2-Iodo-1,3-dimethylbenzene

One 250ml flask was charged with 4-phenyl imidazole (7.08g, 49.12mmole), 2-iodo-m- xylene(9.5g, 40.93mmole), copper (5.721g, 90.046mmole); 18-crown-6 (1.081g, 4.09 mmole), K2CO3 (21.49g, 155.53 mmole) and tetrahydronaphthalene (90ml). Reaction was heated to 180 C for 68hrs. Reaction mixture was then filtered through Celite and the filtrate was concentrated to dryness. The residue was subjected to kugelrohr distillation and 4g of ligand was obtained.(39%).

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; UNIVERSAL DISPLAY CORPORATION; WO2008/54584; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 42861-71-2, The chemical industry reduces the impact on the environment during synthesis 42861-71-2, name is 3-Iodophenyl acetate, I believe this compound will play a more active role in future production and life.

Example 68; 3 -(2- {6-[(3»S)-3 -(2-Fluorophenoxy)azolan- 1 -yl] -3 -pyridazinyl } – 1 -ethynyl)phenyl acetate; Prepared by Sonagashira coupling reaction of Intermediate 20 with 3-iodophenyl acetate in a mixture of DMSO and triethylamine to give the product as a white solid; IR (PCBr) 2938, 2208, 1762, 1578, 1504, 1371, 1240, 1109, 758 cm”1; 1H NMR (300 MHz, CDCl3) delta 2.26 (br s, IH), 2.30 (s, 3H), 2.48 (br s, IH), 3.76-4.02 (m, 4H), 5.11 (br s, IH), 6.61 (d, J= 9.3 Hz, IH), 6.94-7.10 (m, 4H), 7.29-7.36 (m, 4H), 7.42 (d, J = 9.3 Hz, IH); ESI-MS (m/z) 418.12 (M+H)+.

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, 3-Iodophenyl acetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; WO2008/62276; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

These common heterocyclic compound, 672293-33-3, name is Methyl 4-amino-5-iodo-2-methylbenzoate, 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. COA of Formula: C9H10INO2

[0069] Methyl (2-(l-oxopeutyl)-3-(2-phenylethyl)-6-methyl)indole-5-carboxyIate (7); Amixture of 4 (250 mg), l-triethylsilyl-4-phenylbutyne (5, 320 mg), palladium acetate (30 mg), sodium carbonate (450 mg), and degassed DMF (2 mL) was stirred at 100C under argon atmosphere for 5 hours. The reaction mixture was filtered through fluorisil, eluted with 20% ethyl acetate/hexanes and evaporated to afford indole 6 as an amorphous. To a mixture of 6, dichloromethane (3 mL) and valeryl chloride (0.52 mL), zinc chloride (1M in diethyl ether solution, 0.77 mL) was added slowly at 4C, and stirred at 4C for 3 hours. The reaction mixture was treated with methanol (3 mL), diluted with ethyl acetate (30 mL), washed with water twice (10 mL each), aqueous sodium carbonate (10 mL) followed by brine (10 mL), dried (Na2S04), and evaporated. The crude residue was washed with hexanes to give 7 (165 mg) as a brown solid. Mp 145-147C; ]H NMR (CDC13, 400 MHz) 8 8.87 (s, 1H), 8.32 (s, 1H), 7.30-7.20 (m, 3H), 7.19 (s, 1H), 7.14 (d, J= 7.6 Hz, 2H), 3.93 (s, 3H), 3.39 (t, J= 8.4 Hz, 2H), 3.01 (t, J= 7.2 Hz, 2H), 2.74 (t, J= 7.6 Hz, 2H), 2.71 (s, 3H), 1.68 (quintet, J= 7.6 Hz, 2H), 1.68 (dt, J= 7.6 Hz, 15.2 Hz, 2H), 0.95 (t, J= 7.2 Hz, 3H).

The synthetic route of Methyl 4-amino-5-iodo-2-methylbenzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; WO2006/7542; (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. 626-62-0, name is Iodocyclohexane, A new synthetic method of this compound is introduced below., COA of Formula: C6H11I

A mixture of zinc dust (16.34 g, 250 mmol, Aldrich, -325 mesh) and dry tetrahydrofuran (6 mL) under argon was treated with 1,2-dibromoethane (0.94 g, 5 mmol). The zinc suspension was then heated with a heat gun to ebullition, allowed to cool, and heated again. This process was repeated three times to make sure the zinc dust was activated. The activated zinc dust suspension was then treated with trimethylsilyl chloride (0.54 g, 5 mmol), and the suspension was stirred for 15 min at 25 C. The reaction mixture was then treated dropwise with a solution of cyclohexyl iodide (21 g, 100 mmol) in dry tetrahydrofuran (30 mL) over 15 min. During the addition, the temperature rose to 60 C. The reaction mixture was then stirred for 3 h at 40-45 C. The reaction mixture was then cooled to 25 C. and diluted with dry tetrahydrofuran (60 mL). The stirring was stopped to allow the excess zinc dust to settle down (3 h). In a separate reaction flask, a mixture of lithium chloride (8.48 g, 200 mmol, predried at 130 C. under high vacuum for 3 h) and copper cyanide (8.95 g, 100 mmol) in dry tetrahydrofuran (110 mL) was stirred for 10 min at 25 C. to obtain a clear solution. The reaction mixture was cooled to -70 C. and then slowly treated with the freshly prepared zinc solution using a syringe. After the addition, the reaction mixture was allowed to warm to 0 C. where it was stirred for 5 min. The reaction mixture was again cooled back to -70 C. and then slowly treated with methyl propiolate (7.56 g, 90 mmol). The resulting reaction mixture was stirred for 15 h at -70 C. to -50 C. and then slowly treated with a solution of iodine (34.26 g, 135 mmol) in dry tetrahydrofuran (30 mL), with the temperature kept at -70 C. to -60 C. After addition of the iodine solution, the cooling bath was removed, and the reaction mixture was allowed to warm to 25 C. where it was stirred for 2 h. The reaction mixture was then poured into a solution consisting of a saturated aqueous ammonium chloride solution (400 mL) and ammonium hydroxide (100 mL), and the organic compound was extracted into ethyl acetate (3250 mL). The combined organic extracts were successively washed with a saturated aqueous sodium thiosulfate solution (1500 mL) and a saturated aqueous sodium chloride solution (1500 mL), dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 230-400 mesh, 9/1 hexanes/diethyl ether) afforded (E)-3-cyclohexyl-2-iodo-acrylic acid methyl ester (26.3 g, 99%) as a light pink oil: EI-IIRMS m/e calcd for C10H15IO2 (M+) 294.0117, found 294.0114.

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; Hoffmann-La Roche Inc.; US6353111; (2002); 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., Recommanded Product: 1,1,1-Trifluoro-3-iodopropane

a) rac-2-(3-Chloro-phenyl)-5,5,5-trifluoro-pentanoic acid To a stirred solution of m-chlorophenylacetic acid (2.38 g, 14 mmol) in tetrahydrofuran (85 ml) was added at -78 0C lithium diisopropylamide solution (31 ml IM in THF, 31 mmol). After stirring the mixture for 20 min l-iodo-3,3,3-trifluoropropane (4.38 g, 20 mmol) was added and the mixture was allowed to warm to room temperature overnight. Water (5 ml) was added followed by 2N hydrochloric acid (10 ml). The reaction mixture was extracted twice with ethyl acetate. The combined organic layers were dried over MgSCU and evaporated and the residue was purified by column chromatography (Sitheta2, heptane/EtOAc= 9:1) to yield a colourless oil, (1.75 g, 47 %); MS (EI): 264.9 (M+ ).

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; F. HOFFMANN-LA ROCHE AG; WO2008/92785; (2008); 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. 160938-18-1, name is 4-Chloro-2-iodo-1-nitrobenzene, A new synthetic method of this compound is introduced below., Formula: C6H3ClINO2

4-chloro-2-iodo-1-nitrobenzene (77.66 g, 274 mmol), 9-phenyl-9H-carbazol- 2- ylboronic acid (157.34 g, 548 mmol), NaOH (5.48 g, After THF / H2O (800 ml / 400 ml) was mixed, Pd (PPh3) 4 (4.36 g, 5 mol%) was added at 40 C At 80 CStir for 12 hours.After completion of the reaction, the reaction mixture was extracted with methylene chloride, and then MgSO 4 was added thereto, followed by filtration to obtain an organic layer. In the obtained organic layer,The residue was purified by column chromatography (Hexane: EA = 3: 1 (v / v)) to give 2- (5-chloro-2-nitrophenyl) -9-phenyl-9H-carbazole (114.8 g, yield 73%).

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; DoosanCorporation; Kim, Tae Hyung; Han, Song Eii; Lee, Chang Jun; Sin, Jin Yong; Jo, Hyun Jong; Baek, Young Mi; (56 pag.)KR2015/47858; (2015); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 135050-44-1, 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. 135050-44-1, name is 3-Chloro-4-iodoaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

STEP A: 2,4′-dichloro-2′-methyl-[1,1′-biphenyl]-4-amine 3-Chloro-4-iodoaniline (3.0 g, 11.8 mmol), (4-chloro-2-methylphenyl)boronic acid (2.4 g, 14.2 mmol), Pd(dppf)Cl2 (1.0 g, 1.2 mmol), and K2CO3 (3.3 g, 23.7 mmol) were dissolved in 1,4-dioxane (40 mL) and water (10 mL) and the resulting mixture was heated to 80 C. After 16 h the resulting mixture was cooled to room temperature, diluted with EtOAc, washed with water and brine, dried (Na2SO4), and dry packed onto silica gel. Column chromatography yielded the title compound.

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, 3-Chloro-4-iodoaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Chakravarty, Devraj; Greco, Michael; Shook, Brian; Xu, Guozhang; Zhang, Rui; US2012/302641; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com